反应详情

温度

-10 °C

To a stirred suspension of 4-amino-5-chloro-2-ethoxybenzoic acid (2.9 g) in dichloromethane (50 ml), triethylamine (1.6 g) is added at 25° C. The resulting mixture is cooled to -10° C., and isobutyl chloroformate (2.0 g) is added slowly. After the mixture is stirred at the same temperature for 1 hour, a solution of 2-aminomethyl-4-(4-fluorobenzyl)morpholine (3.0 g) in dichloromethane (10 ml) is added. The reaction mixture is stirred for 1 hour at a temperature of between -10° C. and -5° C. and then at 25° C. overnight. The mixture is washed successively with water, 10% aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and evaporated under reduced pressure. The residue is recyrstallized from ethanol to give the title compound (4.1 g), mp 151°-153° C.

1. additionis added at 25° C
2. stirringThe reaction mixture is stirred for 1 hour at a temperature of between -10° C. and -5° C.
3. customat 25° C.
4. customovernight
5. washThe mixture is washed successively with water, 10% aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customevaporated under reduced pressure