HRID4991

反应详情

EQUATION

反应方程式

HRID 4991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

212.6 Grams of 4,6-dimethyl-2-(2-phenylacetyl)-phenol was dissolved in 350 ml of N,N,N',N'-tetramethyldiaminomethane, then under ice-cooled condition with stirring, 350 ml of acetic anhydride was added dropwise thereto. The reaction mixture was further stirred at room temperature for 2 hours, then was poured in 1 kg of ice and stirred vigorously. The crystals separated in the mixture were collected by filtration, washes with water, then dried. Recrystallized from ethanol to obtain 186 g of 2,4-dimethyl-6-(2-phenylacryloyl)phenol. Colorless needle-like crystals. Melting point: 83°-84° C.

WORKUP

后处理

  1. temperatureunder ice-cooled condition
  2. stirringThe reaction mixture was further stirred at room temperature for 2 hours
  3. stirringstirred vigorously
  4. customThe crystals separated in the mixture
  5. filtrationwere collected by filtration, washes with water
  6. customdried
  7. customRecrystallized from ethanol