C07C213/10

Preparation method for high purity racemic adrenaline

Disclosed is a preparation method for a racemic adrenaline as represented by formula II. The method comprises the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95 C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20 C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20 C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method of the present invention is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero; the invention is inexpensive, simple to operate, favors industrialized production, and has a broad application prospect.

Preparation method for high purity racemic adrenaline

Disclosed is a preparation method for a racemic adrenaline as represented by formula II. The method comprises the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95 C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20 C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20 C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method of the present invention is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero; the invention is inexpensive, simple to operate, favors industrialized production, and has a broad application prospect.

METHOD FOR THE PRODUCTION OF ETHYLENEAMINES
20200308097 · 2020-10-01 ·

The present invention relates to a process for purifying a mixture comprising MEG, MEA, EDA and DETA, and low boilers having a boiling point not higher than PIP and high boilers having a boiling point not lower than AEEA, wherein the process comprises the following steps: a) separating a mixture comprising MEG, MEA, EDA and DETA, and low boilers having a boiling point not higher than PIP and high boilers having a boiling point not lower than AEEA, into (i) a mixture A comprising EDA and the low boilers having a boiling point not higher than PIP; and (ii) a mixture B comprising MEA; and (iii) a mixture C comprising MEG, DETA and the high boilers having a boiling point not lower than AEEA; b) separating mixture C from stage a) into (i) a mixture D comprising MEG; and (ii) a mixture E comprising MEG, DETA and the high boilers having a boiling point not lower than AEEA; c) separating mixture E from stage b) either into (i) a mixture F comprising MEG and DETA; and (ii) a mixture G comprising the high boilers having a boiling point not lower than AEEA; or into (i) a mixture F comprising MEG and DETA; and (ii) a mixture G1 comprising AEEA; and (iii) a mixture G2 comprising the high boilers having a boiling point higher than AEEA; d) separating mixture F from stage c) by extractive distillation with triethylene glycol into (i) a mixture H comprising MEG; and (ii) a mixture I comprising DETA and TEG.

METHOD FOR THE PRODUCTION OF ETHYLENEAMINES
20200308097 · 2020-10-01 ·

The present invention relates to a process for purifying a mixture comprising MEG, MEA, EDA and DETA, and low boilers having a boiling point not higher than PIP and high boilers having a boiling point not lower than AEEA, wherein the process comprises the following steps: a) separating a mixture comprising MEG, MEA, EDA and DETA, and low boilers having a boiling point not higher than PIP and high boilers having a boiling point not lower than AEEA, into (i) a mixture A comprising EDA and the low boilers having a boiling point not higher than PIP; and (ii) a mixture B comprising MEA; and (iii) a mixture C comprising MEG, DETA and the high boilers having a boiling point not lower than AEEA; b) separating mixture C from stage a) into (i) a mixture D comprising MEG; and (ii) a mixture E comprising MEG, DETA and the high boilers having a boiling point not lower than AEEA; c) separating mixture E from stage b) either into (i) a mixture F comprising MEG and DETA; and (ii) a mixture G comprising the high boilers having a boiling point not lower than AEEA; or into (i) a mixture F comprising MEG and DETA; and (ii) a mixture G1 comprising AEEA; and (iii) a mixture G2 comprising the high boilers having a boiling point higher than AEEA; d) separating mixture F from stage c) by extractive distillation with triethylene glycol into (i) a mixture H comprising MEG; and (ii) a mixture I comprising DETA and TEG.

Process for preparation of O-Desmethyltramadol and salts thereof

A process of preparation of O-Desmethyl tramadol through potassium hydroxide mediated demethylation of Tramadol under phase transfer conditions.

Process for preparation of O-Desmethyltramadol and salts thereof

A process of preparation of O-Desmethyl tramadol through potassium hydroxide mediated demethylation of Tramadol under phase transfer conditions.

Process for preparation of isoproterenol hydrochloride

The present invention provides a process for preparation of isoproterenol hydrochloride (1a) comprising catalytic hydrogenation of 3,4-dihydroxy-2-(isopropylamino)-acetophenone hydrochloride (5a) in presence of an ion exchange resin, to provide isoproterenol hydrochloride (1a).

Process for preparation of isoproterenol hydrochloride

The present invention provides a process for preparation of isoproterenol hydrochloride (1a) comprising catalytic hydrogenation of 3,4-dihydroxy-2-(isopropylamino)-acetophenone hydrochloride (5a) in presence of an ion exchange resin, to provide isoproterenol hydrochloride (1a).

PREPARATION METHOD FOR HIGH PURITY RACEMIC ADRENALINE
20200270199 · 2020-08-27 ·

A preparation method for a racemic adrenaline as represented by formula II. The method may comprise the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95 C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20 C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20 C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero.

PREPARATION METHOD FOR HIGH PURITY RACEMIC ADRENALINE
20200270199 · 2020-08-27 ·

A preparation method for a racemic adrenaline as represented by formula II. The method may comprise the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95 C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20 C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20 C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero.