HRID464915

反应详情

EQUATION

反应方程式

HRID 464915 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.52 g of 2-pyridinylsulfonamide and 0.55 g of 1,8-diazabicyclo[5.4.0]undec-7-ene in 10 ml of absolute dioxan is added 1 g of N-(4-difluoromethoxy-6-methylpyrimidin-2-yl)-phenylcarbamate. The reaction mixture is stirred for 6 hours at 20°-25° C., then taken up in water and acidified with 2N hydrochloric acid. The precipitate is isolated, washed with water and recrystallised from a mixture of acetone/ether, affording 0.5 g (42.4%) of N-(2-pyridinylsulfonyl)-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)urea (compound 1.1) with a melting point of 150°-151° C.

WORKUP

后处理

  1. customThe precipitate is isolated
  2. washwashed with water
  3. customrecrystallised from a mixture of acetone/ether