HRID2049494

反应详情

EQUATION

反应方程式

HRID 2049494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml of ethanol, 20.3 g (0.3 mole) of methylamine hydrochloride and 30.9 g (0.36 mole) of 37% formaldehyde aqueous solution were added and the mixture was warmed to 35°-40° C. Then, a solution prepared by dissolving 30.9 g (0.3 mole) of isopropyl carbamate in 150 ml of ethanol was added dropwise to the mixture with stirring maintaining the said temperature. After the dropwise addition of the solution, stirring was continued for 1 hour with heating and then the solvent was removed by distillation under reduced pressure. The residue was recrystallized from ethanol to give 42.7 g of isopropyl N-(methylaminomethyl)carbamate hydrochloride having a melting point of 163°-164° C. in yield of 77.8%. ##STR5##

WORKUP

后处理

  1. temperaturethe mixture was warmed to 35°-40° C
  2. customThen, a solution prepared
  3. additionwas added dropwise to the mixture
  4. temperaturemaintaining the said temperature
  5. additionAfter the dropwise addition of the solution
  6. stirringstirring
  7. temperaturewith heating
  8. customthe solvent was removed by distillation under reduced pressure
  9. customThe residue was recrystallized from ethanol