HRID1246326

反应详情

EQUATION

反应方程式

HRID 1246326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 4-butyloxy-3,5-dimethoxybenzoic acid (5.0 g, 0.0197 mol) and thionyl chloride (10 mL) in toluene (10 mL) was heated at 90° C. for 18 h. The reaction mixture was concentrated under reduced pressure. To remove excess of thionyl chloride the residue was repeatedly redissolved in toluene (3×20 mL) and the resulting solution evaporated to dryness to obtain 4-butyloxy-3,5-dimethoxybenzoyl chloride (5.3 g, 99% yield) as a pale yellow oil. 1H NMR (CDCl3) δ: 0.99 (t, J=5.0 Hz, 3H), 1.47 (m, 2H), 1.73 (m, 2H), 3.90 (s, 6H), 4.09 (t, J=5.1 Hz, 2H), 7.36 (s, 2H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customTo remove excess of thionyl chloride the residue
  3. dissolutionwas repeatedly redissolved in toluene (3×20 mL)
  4. customthe resulting solution evaporated to dryness