HRID253267

反应详情

EQUATION

反应方程式

HRID 253267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-hydroxy-4-(methyloxy)benzoate (27 g, 149 mmol.) was taken into acetic anhydride (150 mL) followed by addition of sodium acetate (24 g, 298 mmol.) and the resulting mixture was stirred at room temperature over 20 hours. The solid was filtered and washed once with ethyl acetate and the combined organic layers concentrated in vacuo to a slurry. The solid was collected by filtration, washed once with water and dried in vacuo to provide methyl 3-(acetyloxy)-4-(methyloxy)benzoate (25.9 g, 77% yield) as a white solid. 1H NMR (400 MHz, CDCl3): 7.92 (dd, 1H), 7.70 (d, 1H), 6.97 (d, 1H), 3.88 (s, 3H), 3.87 (s, 3H), 2.32 (s, 3H).

WORKUP

后处理

  1. filtrationThe solid was filtered
  2. washwashed once with ethyl acetate
  3. concentrationthe combined organic layers concentrated in vacuo to a slurry
  4. filtrationThe solid was collected by filtration
  5. washwashed once with water
  6. customdried in vacuo