HRID1588179

反应详情

EQUATION

反应方程式

HRID 1588179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The following are added in succession to a mixture of 2.75 g of 3-n-butylaminopyridin-2-ylsulfonamide in 40 ml of acetonitrile: 3.5 g of phenyl N-(4,6-dimethoxypyrimidin-2-yl)carbamate and 1.97 ml of 1,5-diazabicyclo[5.4.0]undec-5-ene. The reaction mixture is stirred for 30 minutes and evaporated, the oily residue is triturated with 10 ml of 2N hydrochloric acid and subsequently with 10 ml of ice/water and a little diethyl ether, and the mixture is filtered. The filter residue is subsequently washed with a little water and diethyl ether and dried. 4.39 g of N-(3-n-butylaminopyridin-2-ylsulfonyl)-N'-(4,6-dimethoxypyrimidin-2-yl)urea (compound No. 1.001) of a melting point of 118°-119° C. are obtained.

WORKUP

后处理

  1. customevaporated
  2. customthe oily residue is triturated with 10 ml of 2N hydrochloric acid and subsequently with 10 ml of ice/water
  3. filtrationa little diethyl ether, and the mixture is filtered
  4. washThe filter residue is subsequently washed with a little water and diethyl ether
  5. customdried
  6. custom1.001) of a melting point of 118°-119° C. are obtained