HRID2225958

反应详情

EQUATION

反应方程式

HRID 2225958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 40 g of p-toluenesulfonic acid monohydrate and 313 g of diethyl butylmethylmalonate was heated to 125°-135° C. in a flask equipped with a distillation column packed with Raschig rings. After 15 minutes, ethanol began to reflux in the distillation head. Ethanol was distilled as it formed and the pot temperature was maintained at 120°-126° C. by periodic addition of water to the pot. After 22 hours, the distillation of ethanol had ceased. The mixture then was cooled and treated with 70 ml of water. The layers were separated to afford 159.2 g (90.6% yield) of 2-methylhexanoic acid (99.8% pure by VPC).

WORKUP

后处理

  1. temperaturewas heated to 125°-135° C. in a flask
  2. customequipped with a distillation column
  3. temperatureto reflux in the distillation head
  4. distillationEthanol was distilled as it
  5. customformed
  6. waitAfter 22 hours
  7. distillationthe distillation of ethanol
  8. temperatureThe mixture then was cooled
  9. additiontreated with 70 ml of water
  10. customThe layers were separated