Category: 10297-05-9

Related Products of 10297-05-9,Some common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, molecular formula is C4H8ClI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 23: 2-[5-Chloro-1-[(4-chlorophenyl)sulfonyl]pentyl]-1,4-difluorobenzene Under an argon atmosphere and at -78°C, n-butyl lithium (a 1.57M hexane solution, 3.52 ml) was added to a dimethoxyethane solution (30 ml) of the 2-[(4-chlorophenyl)sulfonylmethyl]-1,4-difluorobenzene (1.52 g, 5.02 mmol) obtained in Example 5.. The temperature of the reaction mixture was elevated to room temperature, at which stirring was conducted for 15 minutes.. After cooling the reaction mixture to -78°C, 4-chloro-1-iodobutane (672 mul, 5.52 mmol) was added thereto and the mixture was stirred at room temperature for 24 hours.. A saturated ammonium chloride solution was added to the reaction mixture, followed by extraction with diethyl ether.. The extracts were combined, washed successively with water, a saturated aqueous solution of sodium thiosulfate and brine, dried over MgSO4, and then distilled under reduced pressure to remove the solvent.. The residue thus obtained was recrystallized from hexane, whereby the title compound (1.64 g, 83percent) was obtained as colorless needle crystals. IR (ATR) nu: 2945, 1583, 1495, 1475, 1311, 1277, 1230, 1149, 1142, 1082, 1014, 872, 822, 793, 752, 708, 629, 557, 532, 465 cm-1.1H-NMR (400MHz, CDCl3) delta: 1.33-1.48(2H,m), 1.72-1.87(2H,m), 2.08-2.18(1H,m), 2.43-2.52(1H,m), 3.44-3.53(2H,m), 4.52(1H,ddd,J=11.5,3.9,1.2Hz), 6.84(1H,td,J=9.0,4.4Hz), 6.96-7.02(1H,m), 7.23-7.28(1H,m), 7.39(2H,d,J=8.8Hz), 7.53(2H,d,J=8.8Hz). MS (m/z): 393 (M++H). Elemental Analysis for C17H16Cl2F2O2S Calculated: C 51.92percent; H 4.10percent; Cl 18.03percent; F 9.66percent; S 8.15percent. Found: C 51.33percent; H 4.07percent; Cl 17.64percent; F 9.72percent; S 8.25percent.

The synthetic route of 10297-05-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1466898; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 10297-05-9, name is 1-Chloro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C4H8ClI

(Step 2) [1-(2-Hydroxyethyl)imidazolidin-2-ylidene] malononitrile (2.00 g, 11.2 mmol) obtained in the Step 1 was dissolved in DMF (20 mL) and the solution was sequentially added with potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol). After stirring the mixture at room temperature for 71 hours, potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol) were added, followed by stirring at 35°C for 6 hours and at a room temperature for 14 hours. The mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with diisopropylether to obtain [1-(4-chlorobutyl)-3-(2-hydroxyethyl)imidazolidin-2-ylidene]malononitrile (2.55 g, 84.6percent) as a white solid. 1H NMR (CDCl3, deltappm): 1.87-1.99 (m, 2H), 2.12-2.24 (m, 2H), 3.61-3.76 (m, 12H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 10297-05-9.

Reference:
Patent; KYOWA HAKKO KOGYO CO., LTD.; EP1847530; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 10297-05-9, name is 1-Chloro-4-iodobutane, A new synthetic method of this compound is introduced below., name: 1-Chloro-4-iodobutane

817 mg (4.041 mmol) of 5-hydroxypsoralen and 1.413 g (6.47 mmol) of 4-chlorobutyl iodide were refluxed in 80 ml of acetone in the presence of an excess of (3.0 g) anhydrous potassium carbonate for 30 hours. The progress of the reaction was monitored by thin layer chromatography. After 30 hours the reaction mixture was concentrated under reduced pressure and distilled off the solvent almost completely. The oily residue was cooled and diluted with water. The aqueous solution was then acidified with concentrated hydrochloric acid to pH 1. The slurry was stirred for 15-20 min and extracted with 3.x.100 ml of dichloromethane. The dichloromethane layer was extracted with 1.x.25 ml of 1percent sodium hydroxide to separate trace amounts of un-reacted 5-hydroxypsoralen. The dichloromethane layer was washed with 30 ml of 2percent hydrochloric acid and further washed with water to neutral pH. The dichloromethane layer was dried over anhydrous sodium sulfate and concentrated to dryness. The resulting residue was then suspended in petroleum ether and filtered to wash out the excess 4-chlorobutyl iodide. The resulting 5-(4-chlorobutoxy)psoralen was used for the synthesis of various derivatives without further purification. Yield: 1.10 g (92.98percent) Melting point: 115.4-115.6° C. 1H-NMR (500 MHz, CDCl3): delta [ppm]=8.15 (d, 1H, 3J=9.75 Hz, 3-H), 7.60 (d, 1H, 3J=2.62 Hz, 2′-H), 7.17(s, 1H, 8-H), 6.95 (d, 1H, 3J=2.15 Hz, 3′-H), 6.29 (d, 1H, 3J=9.79 Hz, 4-H), 4.52 (t, 2H, 3J=5.44 Hz, 5-OCH2CH2CH2CH2Cl), 3.68 (t, 2H, 3J=5.89 Hz, 5-OCH2CH2CH2CH2Cl), 2.08 (p, 4H, 3J=3.06 Hz, 5-OCH2CH2CH2CH2Cl).; 500 mg (2.473 mmol) of 5-hydroxypsoralen and 893 mg (4.088 mmol) of 4-iodo-1-chlorobutane were stirred at 25° C. in 30 ml of anhydrous acetone in the presence of an excess (2.0 g) of anhydrous potassium carbonate for 28 hours. The progress of the reaction was monitored by thin layer chromatography. After 28 hours the reaction mixture was concentrated under reduced pressure and distilled off the solvent almost completely. The oily residue was cooled and diluted with water. The aqueous solution was then acidified with concentrated hydrochloric acid to pH 1. The slurry was stirred for 15-20 min and filtered. The solids were washed with water to neutral pH and dried. The dried solids were suspended in petroleum ether, filtered and dried under vacuum.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; The Regents of the University of California; US2006/79535; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 10297-05-9, These common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

EXAMPLE 1503-(2-isopropylphenyl)-5-(4-morpholin-4-ylbutoxy)-l -(3-( 1 -naphthyloxy)propyl)- 1 H-indole-2-carboxylic acidA mixture of EXAMPLE 149A (36 mg), l-chloro-4-iodobutane (0.043 ml) and cesium carbonate (116 mg) in N,N-dimethylformamide (2 ml) was stirred at room temperature overnight. The inorganic salt was filtered off. To the N,N-dimethylformamide solution was added morpholine (0.2 ml) and the resulting mixture was heated at 600C for 5 hours. The reaction mixture was concentrated and the residue was purified by RPHPLC (mobile phase: 10percent-100percent acetonitrile in 0.1percent TFA aqueous solution during 60 min) on a C18 column to give ethyl 3-(2-isopropylphenyl)-5-(4-morpholinobutoxy)-l-(3-(naphthalen- l-yloxy)propyl)-lH-indole-2-carboxylate. This ester was hydrolyzed with aqueous NaOH in a mixture of tetrahydrofuran and methanol to provide the title compound. 1H NMR (400 MHz, dimethyl sulfoxide-d6) ? 9.52 (s, IH), 8.20 (d, J=8.29Hz, IH), 7.87 (d, J=7.98Hz, IH), 7.59 (d, J=8.90Hz, IH), 7.43-7.57 (m, 3H), 7.30-7.43 (m, 3H), 7.14-7.23 (m, IH), 7.06 (d, J=7.36Hz, IH), 6.89 (dd, J=9.05, 2.30Hz, IH), 6.85 (d, J=7.67Hz, IH), 6.43 (d, J=2.45Hz, IH), 4.88 (t, J=7.21Hz, 2H), 4.15 (t, J=5.83Hz, 2H), 3.89-4.03 (m, J=I 1.97Hz, 2H), 3.75-3.89 (m, 2H), 3.55-3.70 (m, 2H), 3.07-3.17 (m, 2H), 3.02 (s, br, 2H), 2.61-2.78 (m, 2H), 2.23-2.45 (m, 2H), 1.60-1.85 (m, 4H).

The synthetic route of 10297-05-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT LABORATORIES; WO2008/130970; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 10297-05-9, name is 1-Chloro-4-iodobutane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 10297-05-9, Recommanded Product: 10297-05-9

(Step 2) [1-(3-Hydroxypropyl)imidazolidin-2-ylidene] malononitrile (1.00 g, 5.21 mmol) obtained in the Step 1 was dissolved in DMF (10 mL) and the solution was sequentially added with potassium carbonate (1.44 g, 10.4 mmol) and 1-chloro-4-iodobutane (1.27 mL, 10.4 mmol). After stirring at room temperature for 18 hours, the mixture was added with saturated brine and extractd with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with diisopropylether to obtain [1-(4-chlorobutyl)-3-(3-hydroxypropyl)imidazolidin-2-ylidene]malononitrile (1.35 g, 91.8percent) as a white solid. 1H NMR (CDCl3, deltappm): 1.80-2.00 (m, 6H), 3.53-3.78 (m, 12H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-4-iodobutane, and friends who are interested can also refer to it.

Electric Literature of 10297-05-9,Some common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, molecular formula is C4H8ClI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

4-Chloro-1-(3-pyridyloxy)butane Under a nitrogen atmosphere, a solution of 3-hydroxypyridine (3.50 g, 36.8 mmol) in N,N-dimethylformamide (DMF) (10 mL) was added drop-wise over 5 min to a cold (0-5° C.), stirring slurry of sodium hydride (1.16 g of an 80percent dispersion in mineral oil, 38.6 mmol) in DMF (40 mL). The mixture was allowed to stir and warm to ambient temperature over 1 h. The mixture was then cooled to 0-5° C., and 1-chloro-4-iodobutane (9.67 g, 44.2 mmol) was added drop-wise over 5 min. The resulting dark-brown mixture was stirred at ambient temperature for 2 h. Water (25 mL) was added, followed by saturated NaCl solution (25 mL), and the mixture was extracted with ether (4*50 mL). The combined ether extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 6.89 g (quantitative yield) of an oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-4-iodobutane, its application will become more common.

Reference of 10297-05-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 10297-05-9 name is 1-Chloro-4-iodobutane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

4-Chloro-1-(3-pyridyloxy)butane Under a nitrogen atmosphere, a solution of 3-hydroxypyridine (3.50 g, 36.8 mmol) in N, N-dimethylformamide (DMF) (10 mL) was added drop-wise over 5 min to a cold (0-5° C.), stirring slurry of sodium hydride (1.16 g of an 80percent dispersion in mineral oil, 38.6 mmol) in DMF (40 mL). The mixture was allowed to stir and warm to ambient temperature over 1 h. The mixture was then cooled to 0-5° C., and 1-chloro4-iodobutane (9.67 g, 44.2 mmol) was added drop-wise over 5 min. The resulting dark-brown mixture was stirred at ambient temperature for 2 h. Water (25 mL) was added, followed by saturated NaCl solution (25 mL), and the mixture was extracted with ether (4*50 mL). The combined ether extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 6.89 g (quantitative yield) of an oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-4-iodobutane, and friends who are interested can also refer to it.

Reference of 10297-05-9,Some common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, molecular formula is C4H8ClI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

4-Chloro-1-(3-pyridyloxy)butane Under a nitrogen atmosphere, a solution of 3-hydroxypyridine (3.50 g, 36.8 mmol) in N, N-dimethylformamide (DMF) (10 mL) was added drop-wise over 5 min to a cold (0-5° C.), stirring slurry of sodium hydride (1.16 g of an 80percent dispersion in mineral oil, 38.6 mmol) in DMF (40 mL). The mixture was allowed to stir and warm to ambient temperature over 1 h. The mixture was then cooled to 0-5° C., and 1-chloro-4-iodobutane (9.67 g, 44.2 mmol) was added drop-wise over 5 min. The resulting dark-brown mixture was stirred at ambient temperature for 2 h. Water (25 mL) was added, followed by saturated NaCl solution (25 mL), and the mixture was extracted with ether (4*50 mL). The combined ether extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 6.89 g (quantitative yield) of an oil.

The synthetic route of 10297-05-9 has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 10297-05-9, name is 1-Chloro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

(1) Preparation of 1-(4-chlorobutoxy)-4-iodobenzene To a solution of 4-iodophenol (1.0 g) in acetonitrile (10 mL), cesium carbonate (3.0 g) and 1-chloro-4-iodobutane (1.2 g) were added and the mixture was heated to 100¡ãC, at which it was stirred for 4 hours. The reaction mixture was cooled to room temperature and filtered to remove insoluble materials, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by NH-type silica gel column chromatography (eluding solvent: n-hexane:ethyl acetate = 7:3 to 1:1) to give the titled compound (1.4 g, 99percent) as a brown oil.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 10297-05-9.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP2221298; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 10297-05-9, These common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

First, 1-chloro-4-iodobutane (1.00 g, 4.57 mmol) was dissolved into a mixture solvent of diethyl ether/pentane (2:3) to obtain a concentration of 0.10 M, the resultant mixture was cooled to -78¡ã C. t-butyl lithium (3.690 g, 9.610 mmol, 1.7M solution in pentane) was added gradually to the cooled solution of 1-chloro-4-iodobutane and stirred for 2 hours. 1,5-dichloropentane-3-one (838 mg, 4.580 mmol) dissolved in diethyl ether (8 mL) was added gradually to the reaction mixture. The reaction mixture was stirred for additional 4 hours at -78¡ã C., and then ice water (50 mL) was added to quench the reaction path, followed by extraction with diethyl ether. The organic layer was collected and dried over anhydrous magnesium sulfate and filtered, the solvents were removed under reduced pressure. The obtained crude product was purified by column chromatography using silica gel (hexane:ethyl acetate=5:1) to obtain 820 mg of compound 17 (yield 65percent).1H NMR (CDCl3): delta 3.52 (t, J=6.4 Hz, 6H, CH2Cl), 1.80-1.73 (m, 6H, CH2), 1.56-1.52 (m, 4H, CH2), 1.42 (s, 4H, CH2) ppm. 13C{1H} NMR (CDCl3): delta 73.58, 45.69, 44.95, 38.29, 36.48, 32.94, 26.96, 20.88 ppm.

The synthetic route of 10297-05-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SK ENERGY CO., LTD.; US2012/165549; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com