Category: 6940-76-7

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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., Product Details of 6940-76-7

A solution of LDA in THF/heptane/ethylbenzene (2.0 M, 137 mL, 274 mmol) was added slowly over 90 min to a stirring solution of N,N’-diisopropyl-2,3-butanediimine (20.0 g, 119 mmol) in distilled THF (180 mL) under N2, maintained at -78 C and stirred for an additional 5 h. A solution of 1-chloro-3-iodopropane (57.4 g, 280 mmol) in distilled THF (20 mL) was added over 15 min and the mixture was stirred at -78 C under N2. After 15 h, aqueous HCl (1M, 600 mL) was added and the mixture was allowed to stir at room temperature (RT) for 5 h. THF was removed under reduced pressure, and CH2Cl2 (160mL x 3) was used to extract the product from the remaining aqueous layer. The organic layers were combined and washed with HCl (1M, 60mL), H2O (120 mL) and sat. NaHCO3 (120mL), and the organic layer was then dried over MgSO4. The mixture was filtered and the filtrate was concentrated under reduced pressure to yield a crude orange oil. The oil was purified by distillation (133-137 C/0.08 mmHg) to give 6 (22.5 g, 94.1 mmol, 79%) as a yellow oil. 1H NMR (500 MHz,CDCl3): 3.55 (t, J = 6.3, 4H), 2.79 (t, J = 7.1, 4H), 1.85-1.70 (m, 8H). 13C NMR (125MHz, CDCl3): 198.9, 44.4, 35.1, 31.7, 20.2. ESI-MS: m/z 241 ([M + H]+, calcd for C10H1735Cl37ClO2 , 241.17554).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Related Products of 6940-76-7, A common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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.

To a solution of 2-fluoro-4-iodo-pyridine (7.70 g, 34.53 mmol, 1.00 eq) in tetrahydrofuran (80 mL) was added lithium diisopropylamide (2 M, 20.72 mL, 1.20 eq) at -78 C for 1.5 h. Then the mixture was added a solution of 1-chloro-3-iodo-propane (14.12 g, 69.06 mmol, 7.43 mL, 2.00 eq) in tetrahydrofuran (10 mL) at -78C and stirred for 0.5 h. Then the mixture was warmed to 15 C and stirred for 1 h. The mixture was quenched with saturated ammonium chloride solution (80 mL) and extracted with ethyl acetate (2 x 40 mL). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate and concentrated to give a residue. The residue was purified by column chromatography (petroleum ether: ethyl acetate = 1:0 to 10:1) to give 3-(3-chloropropyl)-2-fluoro-4-iodo-pyridine (9.00 g, 30.05 mmol, 87% yield) as a light yellow oil.1H-NMR (400MHz, CDCl3) d 7.69 (d, J=5.6 Hz, 1H), 7.61 (d, J=5.2 Hz, 1H), 3.61 (t, J=6.4 Hz, 2H), 2.90 – 2.97 (m, 2H), 2.04 – 2.08 (m, 1H), 1.99 – 2.03 (m, 1H).

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; ARVINAS OPERATIONS, INC.; YALE UNIVERSITY; CREW, Andrew P.; HORNBERGER, Keith R.; WANG, Jing; CREWS, Craig M.; JAIME-FIGUEROA, Saul; DONG, Hanqing; QIAN, Yimin; ZIMMERMAN, Kurt; (1451 pag.)WO2020/51564; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 6940-76-7, name is 1-Chloro-3-iodopropane, 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 6940-76-7, COA of Formula: C3H6ClI

General procedure: In a round flask 300 mg (1.18 mmol) of compound 1 are weighed and placed in an inert atmosphere with a magnetic stirrer. Then, 3 ml of dry THF are added and the system is cooled to 0 C. Then 1.2 equivalents of LDA are added and left in an ice bath for 10 minutes. The ice bath is removed and left under constant stirring for 2 hours. The round flask is cooled again to 0 C and 1,3-chloroiodopropane is added using a syringe previously purged with nitrogen. The ice bath is removed and the reaction is followed by TLC until the consumption of the starting material (1). Once the reaction (approximately 2.5 h) is finished, 0.5 ml of a saturated NH4OH solution is added and an extraction with 5 ml of dichloromethane is carried out in triplicate, the organic phase is collected and dried with anhydrous sodium sulfate, once dried the organic phase is distilled under vacuum. The purification is carried out by a chromatographic column using silica gel as a stationary phase and a mixture of Hexane and ethyl acetate in a proportion of 95:5. A pale yellow oil is obtained in all cases.

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Reference:
Article; Xavier Dominguez-Villa, Francisco; Avila-Zarraga, Gustavo; Armenta-Salinas, Concepcion; Tetrahedron Letters; vol. 61; 15; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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. Safety of 1-Chloro-3-iodopropane

EXAMPLE 14 Ethyl 4-(3-chloropropyl)-4-cyano-1-piperidinecarboxylate To a solution of ethyl 4-cyano-1-piperidinecarboxylate (6.0 g) in tetrahydrofuran (120 ml) at -70 C., under nitrogen, was added a solution of lithium diisopropylamide (4.6 g) in tetrahydrofuran (21.5 ml), dropwise, with stirring. The reaction was allowed to warm to -10 C. and after 30 min was recooled to -70 C. A solution of 1-chloro-3-iodopropane (7.4 g) in tetrahydrofuran (20 ml) was added to the mixture over 30 min. The reaction mixture was quenched with water and allowed to warm to ambient temperature. The mixture was extracted with ethyl acetate. The extracts were washed with water, saturated sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was flash chromatographed (silica), eluding with 2:1 heptane/ethyl acetate. The appropriate fractions were collected and concentrated to afford 5.5 g (64%) of product. Analysis: Calculated for C12 H19 ClN2 O2: 55.70%C 7.40%H 10.83%N Found: 55.88%C 7.67%H 10.80%N

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6940-76-7, its application will become more common.

Reference:
Patent; Hoechst Marion Roussel Inc.; US5756743; (1998); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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. SDS of cas: 6940-76-7

a) Freshly prepared LDA (8.97 mmol) was added to a solution of 2-fluoro-3- iodopyridine (2.00 g, 8.97 mmol) in THF (15 mL) cooled at -78 C. After 1 h, 1 – chloro-3-iodopropane (0.96 mL, 8.97 mmol) was added to the anion solution, allowing to reach room temperature (overnight). The reaction volume was reduced to ca. 10 mL and the mixture was poured over EtAcO (60 mL) and washed with water (2 x 20 mL); the organic layer was dried over anhydrous Na2S04 and filtered. After removal of the solvent, the residue was purified by column chromatography on silica gel (2>4% EtAcO/hexanes), affording 1 .88 g of 3-(3-chloropropyl)-2-fluoro-4- iodopyridine [Rf= 0.70 (5% EtAcO/hexanes), colorless oil, 70% yield].LC-MS ESI+ m/z: 300 (M+1 , 98%) (Method 5).1 H-NMR (CDCI3, 250 MHz, ?): 7.70 (d, J= 5.2 Hz, 1 H, ArH); 7.61 (d, J= 5.2 Hz, 1 H, ArH); 3.62 (t, J= 6.5 Hz, 2H); 2.99-2.90 (m, 2H); 2.10-1 .97 (m, 2H

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6940-76-7, its application will become more common.

Reference:
Patent; LABORATORIOS DEL DR. ESTEVE, S.A.; DRACONIS PHARMA, S.L.; ALMIRALL, S.A.; TORRENS JOVER, Andoni; MERCE VIDAL, Ramon; CALDENTEY FRONTERA, Francesc Xavier; RODRIGUEZ GARRIDO, Antonio, David; CARCELLER GONZALEZ, Elena; SALAS SOLANA, Jordi; WO2013/37960; (2013); 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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., Formula: C3H6ClI

To a suspension of NaH (22 mg, 0.85 mmol) in DMF (2.0 mL) was added S1 (305 mg, 0.78 mmol) in DMF (1.5 mL). After 10 min at room temperature, S4a (0.20 mL, 1.53 mmol) was added to this mixture, and the reaction mixture was stirred at room temperature for 6 h, diluted with ether,washed with water and dried over Na2SO4. Purification by FCC (PE/EtOAc, 8 : 1) gave the chloride S5a (344 mg, 94%) as a yellow oil.

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:
Article; Gao, Yan; Shan, Dong; Jia, Yanxing; Tetrahedron; vol. 70; 34; (2014); p. 5136 – 5141;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6940-76-7, These common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, 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.

Intermediate 54-(3~chloropropyl)-tetrahydro-2H-pyran-4-carbonitrile. To a stirred solution of 1 M LiHMDS (25 mL, 25 mmol) in THF (10 mL) at -78 0C was added dropwise a solution of intermediate 4 (2.23 g, 20 mmol) in THF (15 mL) over 10 minutes. After 40 min, l-chloro-3-iodopropane (2.7 mL, 25 mmol) was added at once, stirred at -78 C for 1 h and 4 h room temperature. Then the reaction mixture was diluted with ether (100 mL), washed with water (20 mL) and brine (20 mL), dried (Na2SO4), filtered and concentrated to give yellow oil which was purified by flash column chromatography using 10-30% EtOAc/Hexanes to afford the product intermediate 5 as a colorless liquid (3.737 g, 99%). 1H NMR (500 MHz, CDCl3) delta: 3.97 (2H, dd, J = 11.3, 3.7 Hz), 3.71 (2H, td, J = 12.2, 1.8 Hz), 3.61 (2H, t, J = 6.3 Hz), 2.05-1.98 (2H, m), 1.88 (2H, dd, J = 13.4, 1.8 Hz), 1.77-1.74 (2H, m), 1.65-1.59 (2H, m).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/58646; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

10.16g(50mmol) of 2-(3′,4′ -dimethoxyphenyl)-3-methylbutyronitrile was dissolved in 80ml of anhydrous toluene, and 3.90g(100mmol) of sodium amide was added in fractional amounts while being stirred. After being heated and refluxed at 120 C for 2 hours, the mixture was cooled down to 80C and, with 15.33g(75mmol) of 1-chloro-3-iodopropane added thereto, further stirred at 80 C for 1 hour. After disappearance of the starting material was checked, a small amount of methanol was added to the mixture to decompose excess sodium amide, and the solvent was evaporated out under a vacuum. The residue was extracted with ethyl acetate and then washed with water until it became neutral. The organic layer was filtrated through 1PS filter paper, and then the solvent was evaporated out. The residue was purified by silica gel column chromatography, to give 12.03g(41mmol, 81%) of 5-chloro-2-(3′,4′ -dimethoxyphenyl)-2-isopropylpentanenitrile. 1H-NMR (d, CDCl3):0.82 (3H, d, J=6.7Hz), 1.21 (3H, d, J=6.7Hz), 1.38-1.54 (1H, m), 1.80-1.98 (1H, m), 2.00-2.30 (3H, m), 3.45-3.54 (2H, m), 3.89 (3H, s), 3.90 (3H, s), 6.82-6.96 (3H, m).

The synthetic route of 1-Chloro-3-iodopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shiseido Co., Ltd.; EP1488776; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows.

4-(3-Chloropropyl)-5,7-difluoro-4H-benzo[1,4]oxazin-3-one 5,7-Difluoro-4H-benzo[1,4]oxazin-3-one (0.24 g, 1.3 mmol), Cs2CO3 (1.08 g, 3.3 mmol), and 1-chloro-3-iodopropane (0.296 g, 1.45 mmol) were mixed according to GP2. Purified by column chromatography (SiO2; heptanes/EtOAc, gradient 0 to 30% EtOAc) to give the title compound (0.17 g, 49%). Rf=0.66 (heptanes/EtOAc 1:1); 1H NMR (CDCl3) d 6.67-6.58 (m, 2H), 4.55 (s, 2H), 4.16-4.10 (m, 2H), 3.59-3.52 (m, 2H), 2.21-2.10 (m, 2H).

The chemical industry reduces the impact on the environment during synthesis 1-Chloro-3-iodopropane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Skjaerbaek, Niels; Koch, Kristian Norup; Mikael Friberg, Bo Lennart; Tolf, Bo-Ragnar; US2005/209226; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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. Recommanded Product: 1-Chloro-3-iodopropane

Lithium diisopropylamide in THF (2.0 M; 12 mL, 24 mmol) was added to a mixture of 2-fluoro-3-iodopyridine (Alfa Aesar, 5.0 g, 22 mmol) in THF (50 mL) at -78 C. The solution was stirred at -78 C. for 1 h, then a solution of 1-chloro-3-iodo-propane, (5.0 g, 24 mmol) in 15 mL THF was added dropwise. The reaction mixture was stirred at -78 C. for 30 min., then allowed to warm to room temperature. The reaction mixture was quenched with aq.NH4Cl and extracted with EtOAc. The combined organic extract was dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using CombiFlash apparatus, eluting with 0 to 50% EtOAc/hexanes, to give the sub-title compound (6.2 g, 92%). LCMS calc. for C8H9ClFIN (M+H)+: m/z=299.9. Found: 300.1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6940-76-7, its application will become more common.

Reference:
Patent; INCYTE CORPORATION; Xue, Chu-Biao; Li, Yun-Long; Geng, Hao; Pan, Jun; Wang, Anlai; Zhang, Ke; Yao, Wenqing; Zhang, Fenglei; Zhuo, Jincong; US2014/200227; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com