HRID843374

反应详情

EQUATION

反应方程式

HRID 843374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
17.5 °C

PROCEDURE

实验过程

Sodium carbonate (224 g) and trans-cinnamyl alcohol (200.0 g) were mixed with 2 L of methylene chloride, a slow nitrogen sweep was maintained through the vapor space of the flask and the mixture was cooled to 15-20° C. with a cold water bath. Peracetic acid solution (35%, 381.2 mL) was added over a 3 hour period, maintaining the internal temperature below 25° C. After the peracetic acid addition was complete, the mixture was stirred for 2-3 hours until complete, as shown by HPLC analysis. The mixture was cooled to 10° C. with an ice bath, and a solution of sodium sulfite (160 g) in 1200 ml water was added slowly over 90 minutes, keeping the temperature below 30° C. The phases were separated and the aqueous phase was extracted with methylene chloride (200 mL) to give a solution of the title compound.

WORKUP

后处理

  1. temperaturea slow nitrogen sweep was maintained through the vapor space of the flask
  2. temperaturemaintaining the internal temperature below 25° C
  3. temperatureThe mixture was cooled to 10° C. with an ice bath
  4. customthe temperature below 30° C
  5. customThe phases were separated
  6. extractionthe aqueous phase was extracted with methylene chloride (200 mL)