HRID1682538

反应详情

EQUATION

反应方程式

HRID 1682538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl [6-methyl-4-(3-phenylphenoxy)-5-pyrimidinyl]-acetate (60 g, 0.18 mol) is added in one portion to a solution of t-BuOK (60 g, 0.53 mol) in 1,2-dimethoxyethane (0.51) at -40° C. After 1 hour dimethylformamide-dimethyl sulfate (1:1 adduct, 120 ml) is added at -50° C. The reaction mixture is allowed to warm to room temperature to give a yellow suspension. Addition of ether, washing repeatedly with brine and drying gives the crude methyl α-[4-methyl-6-(3-phenylphenoxy)-5-pyrimidinyl]-β-dimethylaminoacrylate (67 g, 95%) as an oil. 1H-NMR (CDCl3):8.58 (s, 1H); 7.73 (s, 1H); 7.62-7.03 (m, 9H); 3.68 (s, 3H); 2.87 (s, 6H); 2.44 (s, 3H).

WORKUP

后处理

  1. customto give a yellow suspension
  2. washwashing repeatedly with brine
  3. customdrying