HRID227841

反应详情

EQUATION

反应方程式

HRID 227841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 2000-ml, 4-necked flask equipped with a stirrer were introduced 121 g of O-methyl-N-nitroisourea, 907 g of water, 250 g of sodium chloride and 172 g of methylamine hydrochloride, and the resulting material was maintained at 20 degree centigrade. Thereafter, 8 g of sodium hydrogen carbonate was added to the mixture and the mixture was stirred at 20 degree centigrade for 16 hours. Then, while stirring the reaction mixture, 3.5 g of concentrated hydrochloric acid was added to the mixture. After, the reaction mixture was cooled with ice, the precipitated N,O-dimethyl-N′-nitroisourea was collected by filteration, washed with cold water, and then dried. 91 g of an N,O-dimethyl-N′-nitroisourea crystal with a purity of 99% was obtained. The isolated yield was 67%.

WORKUP

后处理

  1. customInto a 2000-ml, 4-necked flask equipped with a stirrer
  2. temperaturethe resulting material was maintained at 20 degree centigrade
  3. additionwas added to the mixture
  4. temperatureAfter, the reaction mixture was cooled with ice
  5. customthe precipitated N,O-dimethyl-N′-nitroisourea was collected by filteration
  6. washwashed with cold water
  7. customdried