HRID1165357

反应详情

EQUATION

反应方程式

HRID 1165357 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Acetyl chloride (35 m, 492 mmol) was added to 1,1-cyclohexanediacetic acid (25 g, 125 mmol) in a round bottom flask and the suspension was heated for 3 hrs. at 60° C. using an oil bath. After about 15 min. the suspension became clear. The reaction was attached to a short path condenser and was heated to 100° C. under vacuum to remove volatile by products. 1HNMR indicated no starting diacid and GC indicated >99% purity. Upon cooling to room temperature the anhydride solidified. 1H NMR (CDCl3): 62.65(s,4H); 1.45(m,10H)

WORKUP

后处理

  1. temperaturethe suspension was heated for 3 hrs
  2. customat 60° C.
  3. customThe reaction was attached to a short path condenser
  4. customto remove volatile by products
  5. temperatureUpon cooling to room temperature the anhydride