HRID653519

反应详情

EQUATION

反应方程式

HRID 653519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.33 g of 3,4-dihydro-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide, 1.84 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene, 3.2 g of N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate and 35 ml of absolute dioxane is stirred for 45 minutes at a temperature of 20° to 25° C. The solvent is destilled off and the oily residue is triturated with ether and 14 ml of 1N hydrochloric acid. The precipitate is separated, washed with water and dried, affording 4.96 g of N-(3,4-dihydro-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea with a melting point of 215°-218° C.

WORKUP

后处理

  1. customthe oily residue is triturated with ether and 14 ml of 1N hydrochloric acid
  2. customThe precipitate is separated
  3. washwashed with water
  4. customdried