Category: 628-21-7

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 628-21-7

Preparation 122 4′-Chlorospiro[cyclopentane-1,5′-pyrrolo[2,3-d]pyrimidin]-6′(7’H)-one Add 4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (0.6 g; 0.0035 mol; 1.0 equiv) in anhydrous THF (20 mL) and cool the reaction to -78 C., under an inert atmosphere. Add drop-wise lithium hexamethyldisilazide (8.8 mL; 0.0088 mol; 2.5 equiv; 1M in THF). Stir at -78 C. for 30 min. Add drop-wise 1,4-diiodobutane (0.56 mL; 0.0042 mol; 1.2 equiv), allow the reaction temperature to reach 0 C. slowly, and stir for 2 h. Then allow the reaction to reach RT and stir for additional 1 h. Quench the reaction with saturated ammonium chloride solution and extract with EA. Wash the organic layer with water, brine, and dry over anhydrous sodium sulfate. Evaporate the organic layer and purify over a 10 g silica column with acetone (5%) in DCM. Pool fractions to give the title compound (0.34 g; 43.09%). H NMR (DMSO-d6):11.68 (1H, s), 8.53 (1H, s), 2.0-2.1 (m, 2H), 1.91-1.99 (m, 6H).

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shepherd, Timothy Alan; Dally, Robert Dean; Joseph, Sajan; US2010/120801; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 628-21-7,Some common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, molecular formula is C4H8I2, 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.

n-Butyl lithium (2.5 M in hexanes, 3.8 mL, 9.5 mmol) was added dropwise over 30 minutes to a stirred suspension of 6-bromoindolin-2-one (preparation 1, 1.00 g, 4.7 mmol) and N,N,N’,N’-tetramethylethylenediamine (1.42 mL, 9.4 mmol) in tetrahydrofuran (20 mL) at – 78 C. The mixture was stirred for 1 hour, then 1,4-diiodobutane (3.11 mL, 23.6 mmol) was added dropwise over 5 minutes. The mixture was warmed to -20 C over a 1 hour period, was stirred for a further hour at this temperature and was then warmed to room temperature. After 3 hours stirring at room temperature, saturated aqueous ammonium chloride solution was added to the reaction and the mixture was extracted with ethyl acetate. The organic layer was washed with water, brine, dried (MgSO4) and evaporated. Purification of the residue by flash chromatography (10:1 hexanes/ethyl acetate) gave the title compound (0.57 g, 45%) as a pale pink solid. LRMS (m/z): 266/268 (M+1)+. 1H-NMR delta (CDCl3): 1.81-2.20 (m, 8H), 7.02-7.06 (m, 2H), 7.14-7.18 (m, 1H), 7.83 (br s, 1H).

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

Reference:
Patent; Laboratorios Almirall, S.A.; EP2113503; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Name is 1,4-Diiodobutane, 628-21-7, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.

5-Bromo-2- (4-methoxybenzyl) -7-methyliso-1-one at 0 C(3.0 grams, 8.7 moles)N, N-dimethylformamide (30mL)To the solution was added sodium hydride (1.043 g, 43.5 moles).The reaction solution was stirred at room temperature for 10 minutes.Then add 1,5-diiodopentane (3.493 g, 11.3 mol),The reaction solution was stirred at room temperature for 4 hours.After the reaction was monitored by TLC, the reaction was quenched with saturated ammonium chloride solution, and the mixture was extracted with ethyl acetate (100 mL x 2). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by flash column chromatography (petroleum ether / ethyl acetate = 1/1) to give the product in the form of an oil (1.97 hag, yield 56.8%).

Statistics shows that 1,4-Diiodobutane is playing an increasingly important role. we look forward to future research findings about 628-21-7.

Reference:
Patent; Nuowosida Pharmaceutical Co., Ltd.; Li Bing; (67 pag.)CN110256432; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, The chemical industry reduces the impact on the environment during synthesis 628-21-7, name is 1,4-Diiodobutane, I believe this compound will play a more active role in future production and life.

Sodium hydride (2.8 g, 60% dispersion in mineral oil) was added slowly to a solution of (4-nitro-phenyl)-acetic acid methyl ester (6.0 g, 30.7 mmol) in anhydrous DMF (30 mL) under nitrogen at a temperature in the range of 0 C. to 10 C. After stirring at a temperature in the range of 0 C. to 10 C. for 20 min, diiodobutane (7.86 mL, 61 mmol) was added drop-wise under stirring. After complete addition, the reaction mixture was warmed to a temperature in the range of 15 C. to 40 C. and stirring continued for an additional 3 hours. The reaction was quenched by adding water slowly. The mixture was extracted by ethyl acetate (3¡Á40 mL). The combined organic extracts were washed with water, brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resultant gummy material was purified by column chromatography over silica gel to afford a pale yellow thick liquid which solidified on standing at a temperature in the range of 15 C. to 40 C. (4.1 g, 54% yield). The solid (3.4 g, 13.6 mmol) was dissolved in anhydrous EtOH and tin chloride dihydrate (13.86 g, 61 mmol) was added slowly under nitrogen. Thereafter, the mixture was heated at 90 C. for 3 hours. After evaporation of volatiles under reduced pressure, the resultant mixture was diluted with ice-water and aqueous sodium hydroxide was added to adjust pH 11. The mixture was extracted with ethyl acetate (3¡Á50 mL). The combined organic extracts were washed with water, brine, dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure to afford the title compound as a granular light yellow solid (2.67 g, 88% yield).1HNMR (CDCl3, 300 MHz): delta 7.16 (dd, J=8.4, 1.8 Hz, 2H), 6.63 (dd, J=8.4, 1.8 Hz, 2H), 3.59 (s, 3H), 2.60-2.55 (m, 2H), 1.87-1.67 (m, 6H).LC-MSD (ES+): (m/z) 220 [(M+H)+, 100].

The chemical industry reduces the impact on the environment during synthesis 628-21-7. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Dr. Reddy’s Laboratories Ltd.; US2010/144731; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, A common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, molecular formula is C4H8I2, 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.

In a 250 mL three-necked flask was added 19.4 g of anthrone (0.1 mol), 150 mL of dry THF, under stirring, 34. 1 g of 1,4-diiodobutane (0.1 1 mol) and 26.8 g of potassium tert-butoxide (0.24 mol) the reaction was stirred at room temperature for 3 h and refluxed for 3 h. The reaction was quenched by the addition of saturated ammonium chloride solution, extracted with ethyl acetate, separated by column chromatography, and 13.6 g of white solid B-I was obtained by column chromatography. The yield was 55%

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kunshan Weixinnuo Display Co., Ltd.; Tsinghua University; Beijing Weixinnuo Technology Co., Ltd.; Qiu Yong; Fan Hongtao; (61 pag.)CN103508940; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Adding a certain compound to certain chemical reactions, such as: 628-21-7, name is 1,4-Diiodobutane, 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 628-21-7.

2-[4-(4-iodobutoxy)phenyl]-1,2-benzisoselenazol-3(2H)-one (Compound 14) To a suspension of NaH (60% emulsion washed with pentane and dried in vacuo, 60 mg, 1.50 mmol) in dry DMF (1 mL) at 0 C. under argon was added a solution of 13 (300 mg, 1.03 mmol) in dry DMF (7 mL) under argon via a cannula. The resultant solution was stirred for 2 hours at room temperature then added via a cannula to a solution of 1,4-diiodobutane (3.20 g, 10.3 mmol) in dry DMF (2 mL) under argon. The resultant solution was stirred in the dark for 2 days at room temperature under argon. Water (1 mL) was carefully added and solvent removed in vacuo to give an oily residue. The residue was dissolved in CH2Cl2 (20 mL) and the organic phase washed with H2O (20 mL), 10% Na2S2O3 (20 mL), and H2O (20 mL). The organic extract was dried over Na2SO4 and filtered. Solvent was removed from the filtrate in vacuo, giving a yellow oily residue. The residue was chromatographed (silica gel packed in CH2Cl2, eluding with 19:1 CH2Cl2/diethyl ether) and fractions containing product were combined. Solvent was removed in vacuo, giving sufficiently pure 14 as a white solid (254 mg, 52%). 1H NMR (299.9 MHz, CDCl3) delta 8.11 (d, J=7.8 Hz, 2H, ArH), 7.68-7.62 (m, 2H, Ar-H), 7.52-7.43 (m, 3H, Ar-H), 6.94 (d, J=9 Hz, 2H, Ar-H), 4.02 (t, J=5.9 Hz, 2H, -O-CH2-), 3.27 (t, J=6.6 Hz, 2H, -CH2-I), 1.98 (m, 4H, -CH2-CH2-); 13C-NMR (125.7 MHz, CDCl3) delta 166.20 (carbonyl), 158.0 (aromatic), 138.12 (aromatic), 132.73 (aromatic), 132.03 (aromatic), 129.73 (aromatic), 127.73 (protonated aromatic), 127.60 (aromatic), 126.85 (aromatic), 126.85 (aromatic), 124.08 (aromatic), 115.41 (protonated aromatic), 67.32 (-O-CH2-), 30.43 (methylene), 6.64 (-CH2-I); LRAPCI MS (+formic acid) Calcd. For C17H17NOSeI: 473, found: 473.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Medical Research Council; University of Otago; US2004/29851; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, These common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, 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.

In three 250ml flask anthrone 19.4g (0.1mol), 150ml dried THF, was added with stirring diiodobutane (34.1g, 0.11mol), potassium tert-butoxide and 26.8g (0.24mol), the reaction was stirred for 3 hours at room temperature, the reaction was refluxed for 3 hours. Saturated ammonium chloride solution was added to quench the reaction, extracted with ethyl acetate, dried liquid separation, column chromatography to obtain 13.6 g of a white solid, a yield of 55%.

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 628-21-7.

Reference:
Patent; KUNSHAN VISIONOX DISPLAY CO., LTD.; BEIJING VISIONOX TECHNOLOGY CO., LTD; Tsinghua University; Qiu, Yong; Fan, Hongtao; Duan, Lian; (49 pag.)CN103172524; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Adding a certain compound to certain chemical reactions, such as: 628-21-7, name is 1,4-Diiodobutane, 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 628-21-7.

To a solution of 500 mg (2.16 mmol) of L-serine benzyl ester hydrochloride and 869 mg (2.81 mmol, 1.3 eq.) of 1,4-diiodobutane in 25 ml of 2-propanol were added, under argon at RT, 595 mg (5.61 mmol, 2.6 eq.) of sodium carbonate and the mixture was stirred at 90 C. overnight. After cooling to RT and removal of the 2-propanol under reduced pressure, the residue was admixed with ethyl acetate. The insoluble salts were filtered off. The filtrate was washed with water and the organic phase was dried (sodium sulphate), filtered and concentrated under reduced pressure. The residue was purified by means of flash chromatography (silica gel 50, dichloromethane, then dichloromethane/methanol 5:1). Yield: 268 mg (48% of theory) LC/MS [Method 5]: Rt=2.03 min; MS (ESIpos): m/z=250 (M+H)+.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; ROeHRIG, Susanne; HILLISCH, Alexander; HEITMEIER, Stefan; SCHMIDT, Martina Victoria; SCHLEMMER, Karl-Heinz; TERSTEEGEN, Adrian; TELLER, Henrik; US2018/346424; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Adding a certain compound to certain chemical reactions, such as: 628-21-7, name is 1,4-Diiodobutane, 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 628-21-7.

Into a 100 ml flask to which a condensing device was connected, 50 ml of acetonitrile, 15.5 g (0.05 mol) of 1,4-diiodobutane and 6.8 g of aqueous ammonia (NH3 0.1 mol) were added. 20C constant temperature stirring reaction 12h. The obtained reaction solution was subjected to cation chromatography. According to the product content in the reaction solution. The yield was calculated to be 85.35%.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Changshu Institute Co., Ltd., East China University of Science and Technology; East China University of Science and Technology; Guan, Shiyou; Feng, Lei; Xiong, Yachao; Yan, Xinzhu; (16 pag.)CN105732645; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

n-Butyl lithium (2.5 M in hexanes, 4.2 mL, 0.5 mmol) was added dropwise to a suspension of indolinone (0.665 mg, 5 mmol) and TMEDA (1.5 mL, 10 mmol) in THF (20 mL) at -78C in a dried flask under nitrogen. After 1 hour at -78C, 1,4- diiodobutane (3.3 mL, 25 mmol) was added dropwise and the mixture was allowed to slowly warm to rt. After 12 hours at rt, saturated aqueous ammonium chloride was added to the mixture and this mixture was extracted with EtOAc. The combined organic phases were washed with water, brine, dried over magnesium sulphate, filtered and concentrated in vacuo. Chromatography on silica (10-30% EtOAc in isohexane) gave isolation of the desired compound as a pale pink solid (393 mg, 2.1 mmol, 42%). ? NMR (400 MHz): delta 1.90 (m, 2H), 2.03 (m, 2H), 2.10 ( m, 2H), 2.21 (m, 2H), 6.94 ( m, 1H), 7.04 ( m, 1H), 7.20 (m, 2H), 8.75 ( bs, 1H). LC/MS 188 (MH+).

The synthetic route of 1,4-Diiodobutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RE:VIRAL LTD; COCKERILL, Stuart; PILKINGTON, Christopher; LUMLEY, James; ANGELL, Richard; MATHEWS, Neil; WO2013/68769; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com