Category: 6306-61-2

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. 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: C5H13Cl2N

KOH (932 mg; 14.1 mmol) was dissolved in THF (7ml) and H20 (distilled, 0.17 ml). Intermediate 7 (341 mg; 0.95 mmol), then tetrabutylammonium bromide (76.5 mg, 0.24 mmol) were added to the mixture and stirred at room temperature for 5 minutes. The reaction mixture was heated at 50C for 1 hour. Then A/-(2-chloroethyl)-2-propanamine, hydrochloride (225 mg, 1.4 mmol) was added and the reaction mixture was stirred at 50C for 18 hours. A/-(2-chloroethyl)-2-propanamine, hydrochloride (76mg, 0.48 mmol) was added and the reaction mixture was stirred at 50C for 5 hours. Water was added and the reaction mixture was extracted with EtOAc. The organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The crude product was purified by chromatography over silica gel (5muetaeta, mobile phase :Gradient from 0.2% NH4OH, 98% DCM, 2% MeOH to 0.8% NH4OH, 92% DCM, 8% MeOH). The desired product fraction was collected and the solvent was evaporated. The residue was dissolved in MeOH, 2 drops of HCI (37%) were added and the reaction mixture was stirred at room temperature for 2 minutes. The mixture was evaporated, taken up with CH3CN and crystallized from CH3CN to afford 41 mg of compound 1 (9%) as a chlorohydrate

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; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; ANGIBAUD, Patrick Rene; WOODHEAD, Steven John; SAXTY, Gordon; WO2013/61074; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, belongs to chlorides-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 6306-61-2, Application In Synthesis of N-(2-Chloroethyl)propan-2-amine hydrochloride

To a stirred mixture of 2-methyltetrahydrofuran (1.5L) and KOH (140g, 250mmol) was added water (30ml_). Then intermediate 3 (60g, 166mmol)) andtetrabutylammoniumbromide (13.4g, 41 mmol) were added and the mixture was heated at 50C for 1 hour while stirring. Then N-(2-chloroethyl)-2-propanamine HCI (CAS[6306- 61 -2]) (48g, 299mmol) was added in 1 portion. The mixture was stirred for 18 hours at 50C. When the conversion was complete, water (600ml_) was added to the reaction mixture. The layers were separated and the organic layer was concentrated. The residue was dissolved in 2-propanol (120ml_) and HCI in 2-propanol was added at 60C. After cooling, the HCI-salt was isolated via filtration. After drying at 50C in a vacuum drying oven the HCI-salt was obtained in 83% yield (compound 4a).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, N-(2-Chloroethyl)propan-2-amine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; SAXTY, Gordon; MURRAY, Christopher William; BERDINI, Valerio; BESONG, Gilbert Ebai; HAMLETT, Christopher Charles Frederick; JOHNSON, Christopher Norbert; WOODHEAD, Steven John; READER, Michael; REES, David Charles; MEVELLEC, Laurence Anne; ANGIBAUD, Patrick Rene; FREYNE, Eddy Jean Edgard; GOVAERTS, Tom Cornelis Hortense; WEERTS, Johan Erwin Edmond; PERERA, Timothy Pietro Suren; GILISSEN, Ronaldus Arnodus Hendrika Joseph; WROBLOWSKI, Berthold; LACRAMPE, Jean Fernand Armand; PAPANIKOS, Alexandra; QUEROLLE, Oliver Alexis Georges; PASQUIER, Elisabeth Therese Jeanne; PILATTE, Isabelle Noelle Constance; BONNET, Pascal Ghislain Andre; EMBRECHTS, Werner Constant Johan; AKKARI, Rhalid; MEERPOEL, Lieven; WO2011/135376; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6306-61-2,Some common heterocyclic compound, 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, molecular formula is C5H13Cl2N, 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 10 (500 mg; 1.26 mmol) then tetrabutylammonium bromide (203.3 mg; 0.63 mmol) were added to a solution of KOH (1.25 g; 18.9 mmol) in 2- methyltetrahydrofuran (15 mL) and water (1 mL) at rt. The reaction mixture was heated at 50C for 1 h, then 2-isopropylaminoethylchloride hydrochloride (CAS 6306- 61-2) (279 mg; 1.77 mmol) was added. The reaction mixture was heated at 50C for 20 hours. The reaction mixture was cooled to rt, then poured into water and brine. EtOAc was added and the organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The residue (0.7 g) was purified by chromatography over silica gel (irregular SiOH, 15-40muetaiota 30g; mobile phase: 0.4% NH4OH, 98% DCM, 2% MeOH). The pure fractions were collected and evaporated to dryness to give 130 mg which was crystallized from Et20 to give 88 mg (14%) of compound 42. MP.: 75C (gum, Kofler).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N-(2-Chloroethyl)propan-2-amine hydrochloride, its application will become more common.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; ANGIBAUD, Patrick Rene; WOODHEAD, Steven John; SAXTY, Gordon; WO2013/61074; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, 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. Formula: C5H13Cl2N

In anhydrous conditions under argon atmosphere, NaH (60% in mineral oil, 0.232 g, 5.8 mmol) was added slowly to a suspension of intermediate 9 (0.35 g, 0.97 mmol) in N,N- dimethylformamide (10 ml) at 0C and the mixture was stirred at 0C for 10 minutes. Isopropylaminoethyl chloride hydrochloride (0.459 g, 2.9 mmol) was added portionwise and the reaction mixture was stirred at room temperature for 48 h ours. The reaction mixture was quenched with a saturated solution of ammonium chloride (15 ml) and the mixture was extracted with ethyl acetate (3 x 50 ml). The combined organic layers were washed with a saturated solution of sodium chloride (2 x 50 ml), dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified bychromatography over silica gel (mobile phase, gradient from 95% DCM, 5%MeOH to 90% DCM, 10%). The fractions were collected and the solvent was evaporated yielding 0.22g of fraction 2 composed of a mixture of compound 4 and compound 6..Fraction 1 and Fraction 2 were combined and purified by achiral SFC (mobile phase, 0.3% isopropylamine, 86% C02, 14% MeOH). The desired fractions were collected and concentrated, yielding 17 mg of compound 5, 168 mg of compound 4 and 60 mg of product fraction 3 containing compound 4 and compound 6..Compound 4 was converted into the HCI salt (3eq. 1 M solution in water) in Et20 and triturated . The precipitate was filtered off, washed with Et20 and dried under vacuum, yielding 153 mg of compound 4 (mp = 175C Kofler).Product fraction 3 was purified by chiral SFC on (5muiotaeta mobile phase, 0.3%isopropylamine, 85% C02, 15% MeOH), yielding 22mg of compound 6.

The synthetic route of N-(2-Chloroethyl)propan-2-amine hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; ANGIBAUD, Patrick Rene; OBRINGER, Michel; MARIN, Julien Jeremie Joseph; JEANTY, Matthieu; WO2013/61077; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, belongs to chlorides-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 6306-61-2, Formula: C5H13Cl2N

To a stirred mixture of 2-methyltetrahydrofuran (1.5L) and KOH (140g, 250mmol) was added water (30ml_). Then intermediate 3 (60g, 166mmol)) andtetrabutylammoniumbromide (13.4g, 41 mmol) were added and the mixture was heated at 50C for 1 hour while stirring. Then N-(2-chloroethyl)-2-propanamine HCI (CAS[6306- 61 -2]) (48g, 299mmol) was added in 1 portion. The mixture was stirred for 18 hours at 50C. When the conversion was complete, water (600ml_) was added to the reaction mixture. The layers were separated and the organic layer was concentrated. The residue was dissolved in 2-propanol (120ml_) and HCI in 2-propanol was added at 60C. After cooling, the HCI-salt was isolated via filtration. After drying at 50C in a vacuum drying oven the HCI-salt was obtained in 83% yield (compound 4a).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, N-(2-Chloroethyl)propan-2-amine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; SAXTY, Gordon; MURRAY, Christopher William; BERDINI, Valerio; BESONG, Gilbert Ebai; HAMLETT, Christopher Charles Frederick; JOHNSON, Christopher Norbert; WOODHEAD, Steven John; READER, Michael; REES, David Charles; MEVELLEC, Laurence Anne; ANGIBAUD, Patrick Rene; FREYNE, Eddy Jean Edgard; GOVAERTS, Tom Cornelis Hortense; WEERTS, Johan Erwin Edmond; PERERA, Timothy Pietro Suren; GILISSEN, Ronaldus Arnodus Hendrika Joseph; WROBLOWSKI, Berthold; LACRAMPE, Jean Fernand Armand; PAPANIKOS, Alexandra; QUEROLLE, Oliver Alexis Georges; PASQUIER, Elisabeth Therese Jeanne; PILATTE, Isabelle Noelle Constance; BONNET, Pascal Ghislain Andre; EMBRECHTS, Werner Constant Johan; AKKARI, Rhalid; MEERPOEL, Lieven; WO2011/135376; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 6306-61-2,Some common heterocyclic compound, 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, molecular formula is C5H13Cl2N, 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 10 (500 mg; 1.26 mmol) then tetrabutylammonium bromide (203.3 mg; 0.63 mmol) were added to a solution of KOH (1.25 g; 18.9 mmol) in 2- methyltetrahydrofuran (15 mL) and water (1 mL) at rt. The reaction mixture was heated at 50C for 1 h, then 2-isopropylaminoethylchloride hydrochloride (CAS 6306- 61-2) (279 mg; 1.77 mmol) was added. The reaction mixture was heated at 50C for 20 hours. The reaction mixture was cooled to rt, then poured into water and brine. EtOAc was added and the organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The residue (0.7 g) was purified by chromatography over silica gel (irregular SiOH, 15-40muetaiota 30g; mobile phase: 0.4% NH4OH, 98% DCM, 2% MeOH). The pure fractions were collected and evaporated to dryness to give 130 mg which was crystallized from Et20 to give 88 mg (14%) of compound 42. MP.: 75C (gum, Kofler).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N-(2-Chloroethyl)propan-2-amine hydrochloride, its application will become more common.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; ANGIBAUD, Patrick Rene; WOODHEAD, Steven John; SAXTY, Gordon; WO2013/61074; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, A new synthetic method of this compound is introduced below., Quality Control of N-(2-Chloroethyl)propan-2-amine hydrochloride

KOH (932 mg; 14.1 mmol) was dissolved in THF (7ml) and H20 (distilled, 0.17 ml). Intermediate 7 (341 mg; 0.95 mmol), then tetrabutylammonium bromide (76.5 mg, 0.24 mmol) were added to the mixture and stirred at room temperature for 5 minutes. The reaction mixture was heated at 50C for 1 hour. Then A/-(2-chloroethyl)-2-propanamine, hydrochloride (225 mg, 1.4 mmol) was added and the reaction mixture was stirred at 50C for 18 hours. A/-(2-chloroethyl)-2-propanamine, hydrochloride (76mg, 0.48 mmol) was added and the reaction mixture was stirred at 50C for 5 hours. Water was added and the reaction mixture was extracted with EtOAc. The organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The crude product was purified by chromatography over silica gel (5muetaeta, mobile phase :Gradient from 0.2% NH4OH, 98% DCM, 2% MeOH to 0.8% NH4OH, 92% DCM, 8% MeOH). The desired product fraction was collected and the solvent was evaporated. The residue was dissolved in MeOH, 2 drops of HCI (37%) were added and the reaction mixture was stirred at room temperature for 2 minutes. The mixture was evaporated, taken up with CH3CN and crystallized from CH3CN to afford 41 mg of compound 1 (9%) as a chlorohydrate

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; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; ANGIBAUD, Patrick Rene; WOODHEAD, Steven John; SAXTY, Gordon; WO2013/61074; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics