N-methyl-3-(methylamino)propanamide;hydrochloride

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 16.1 g of 2-(methyl-chloroacetamido)-5-chlorobenzophenone, 10 g of triethylamine and 7.6 g of 3-methylaminopropionic acid methylamide hydrochloride in 500 ml of anhydrous xylene is heated to reflux for 12 hours whilst stirring. The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling and, after extracting three times by shaking with water, the organic phase is dried over anhydrous potassium carbonate, filtered and evaporated in vacuo. The oily crude base thus obtained (18 g) is dissolved in 800 ml of anhydrous diethyl ether and filtered and 17.0 g of 2-(5-methylaminocarbonyl-N-methyl-3-methyl-3-aza-pentanamido)-5-chlorobenzophenone hydrochloride (77% of theory), with a melting point of 151°-153°, are obtained by passing dry hydrogen chloride into the solution. is heated to reflux for 12 hours The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling after extracting three times by shaking with water the organic phase is dried over anhydrous potassium carbonate filtered evaporated in vacuo The oily crude base thus obtained (18 g) filtered

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 16.1 g of 2-(methyl-chloroacetamido)-5-chlorobenzophenone, 10 g of triethylamine and 7.6 g of 3-methylaminopropionic acid methylamide hydrochloride in 500 ml of anhydrous xylene is heated to reflux for 12 hours whilst stirring. The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling and, after extracting three times by shaking with water, the organic phase is dried over anhydrous potassium carbonate, filtered and evaporated in vacuo. The oily crude base thus obtained (18 g) is dissolved in 800 ml of anhydrous diethyl ether and filtered and 17.0 g of 2-(5-methylaminocarbonyl-N-methyl-3-methyl-3-aza-pentanamido)-5-chlorobenzophenone hydrochloride (77% of theory), with a melting point of 151°-153°, are obtained by passing dry hydrogen chloride into the solution. is heated to reflux for 12 hours The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling after extracting three times by shaking with water the organic phase is dried over anhydrous potassium carbonate filtered evaporated in vacuo The oily crude base thus obtained (18 g) filtered

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 16.1 g of 2-(methyl-chloroacetamido)-5-chlorobenzophenone, 10 g of triethylamine and 7.6 g of 3-methylaminopropionic acid methylamide hydrochloride in 500 ml of anhydrous xylene is heated to reflux for 12 hours whilst stirring. The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling and, after extracting three times by shaking with water, the organic phase is dried over anhydrous potassium carbonate, filtered and evaporated in vacuo. The oily crude base thus obtained (18 g) is dissolved in 800 ml of anhydrous diethyl ether and filtered and 17.0 g of 2-(5-methylaminocarbonyl-N-methyl-3-methyl-3-aza-pentanamido)-5-chlorobenzophenone hydrochloride (77% of theory), with a melting point of 151°-153°, are obtained by passing dry hydrogen chloride into the solution. is heated to reflux for 12 hours The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling after extracting three times by shaking with water the organic phase is dried over anhydrous potassium carbonate filtered evaporated in vacuo The oily crude base thus obtained (18 g) filtered