N,N-二甲基-2-吗啉甲胺盐酸盐

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 22.5 g of 4-benzyl-2-chloromethylmorpholine, 200 ml of ethanol and 200 ml of an aqueouos 26,7% dimethylamine solution is heated at 150° C. for 5 hours in an autoclave. After completion of the reaction, the solvent is distilled off under reduced pressure. After adding water, the residue is extracted with toluene three times. The extract is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled off under reduced pressure and the residue is treated with 37% hydrochloric acid-ethanol to give 2-(N,N-dimethylaminomethyl)-4-benzylmorpholine dihydrochloride as white crystals. A mixture of 22.9 g of the hydrochloride compound, 200 ml of ethanol and 100 ml of water is subjected to catalytic reduction with 2.3 g of 10% palladium-carbon at ordinary temperature and atmospheric pressure. After absorbing a theoretical volume of the hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The obtained residue is treated with ethanol to give 2-(N,N-dimethylaminomethyl)morpholine dihydrochloride as white crystals, melting at 270°-271° C. After absorbing a theoretical volume of the hydrogen the catalyst is filtered off the filtrate is concentrated under reduced pressure The obtained residue is treated with ethanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 22.5 g of 4-benzyl-2-chloromethylmorpholine, 200 ml of ethanol and 200 ml of an aqueouos 26,7% dimethylamine solution is heated at 150° C. for 5 hours in an autoclave. After completion of the reaction, the solvent is distilled off under reduced pressure. After adding water, the residue is extracted with toluene three times. The extract is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled off under reduced pressure and the residue is treated with 37% hydrochloric acid-ethanol to give 2-(N,N-dimethylaminomethyl)-4-benzylmorpholine dihydrochloride as white crystals. A mixture of 22.9 g of the hydrochloride compound, 200 ml of ethanol and 100 ml of water is subjected to catalytic reduction with 2.3 g of 10% palladium-carbon at ordinary temperature and atmospheric pressure. After absorbing a theoretical volume of the hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The obtained residue is treated with ethanol to give 2-(N,N-dimethylaminomethyl)morpholine dihydrochloride as white crystals, melting at 270°-271° C. After absorbing a theoretical volume of the hydrogen the catalyst is filtered off the filtrate is concentrated under reduced pressure The obtained residue is treated with ethanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 22.5 g of 4-benzyl-2-chloromethylmorpholine, 200 ml of ethanol and 200 ml of an aqueouos 26,7% dimethylamine solution is heated at 150° C. for 5 hours in an autoclave. After completion of the reaction, the solvent is distilled off under reduced pressure. After adding water, the residue is extracted with toluene three times. The extract is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled off under reduced pressure and the residue is treated with 37% hydrochloric acid-ethanol to give 2-(N,N-dimethylaminomethyl)-4-benzylmorpholine dihydrochloride as white crystals. A mixture of 22.9 g of the hydrochloride compound, 200 ml of ethanol and 100 ml of water is subjected to catalytic reduction with 2.3 g of 10% palladium-carbon at ordinary temperature and atmospheric pressure. After absorbing a theoretical volume of the hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The obtained residue is treated with ethanol to give 2-(N,N-dimethylaminomethyl)morpholine dihydrochloride as white crystals, melting at 270°-271° C. After absorbing a theoretical volume of the hydrogen the catalyst is filtered off the filtrate is concentrated under reduced pressure The obtained residue is treated with ethanol