HRID1974169

反应详情

EQUATION

反应方程式

HRID 1974169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of magnesium methyl carbonate in dimethyl formamide (300 g of a 2.0 mM/g solution) is heated in a 120° C oil bath with stirring under carbon dioxide flushing for 1/2 hour. To this mixture is added 32.3 g (0.100 mole) of 5-(tetradecyloxy)-2-furyl methyl ketone, and the oil bath temperature is raised to 130° C to 150° C. Dry nitrogen is flushed through the mixture for 5 hours. The mixture is allowed to cool to room temperature under carbon dioxide flushing after which it is poured slowly into 2 liters of concentrated HCl-ice (1:1) with vigorous stirring. When the evolution of gas is complete the precipitate is collected and washed with cold water, then dried to give 2-[5-(tetradecyloxy)-2-furoyl]acetic acid.

WORKUP

后处理

  1. temperaturethe oil bath temperature is raised to 130° C to 150° C
  2. customDry nitrogen is flushed through the mixture for 5 hours
  3. temperatureto cool to room temperature under carbon dioxide flushing after which it
  4. additionis poured slowly into 2 liters of concentrated HCl-ice (1:1) with vigorous stirring
  5. customis collected
  6. washwashed with cold water
  7. customdried