HRID247067

反应详情

EQUATION

反应方程式

HRID 247067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Chloropyrimidin-2-one (5 mmol) and triethylamine (5 mmol) were stirred together in dichloromethane (50 ml). When all the solid had dissolved a solution of chloromethoxybenzene (see Preparation 2) (5 mmol) in dichloromethane (25 ml) was added with stirring at room temperature. The resultant mixture was stirred for 24 h at this temperature before the solvent was distilled off. The residue was triturated with water (30 ml), extracted into chloroform (3×20 ml), and the dried (MgSO4) solution evaporated to yield a mixture of the title compound and the O-alkylated isomer in the ratio 3:1; yield 7.00 g (85%). The N-isomer was separated by column chromatography on silica gel; m.p. 146° C.

WORKUP

后处理

  1. additionwas added
  2. distillationwas distilled off
  3. customThe residue was triturated with water (30 ml)
  4. extractionextracted into chloroform (3×20 ml)
  5. dry with materialthe dried (MgSO4) solution
  6. customevaporated
  7. customto yield