HRID2225958
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated to 125°-135° C. in a flask
- customequipped with a distillation column
- temperatureto reflux in the distillation head
- distillationEthanol was distilled as it
- customformed
- waitAfter 22 hours
- distillationthe distillation of ethanol
- temperatureThe mixture then was cooled
- additiontreated with 70 ml of water
- customThe layers were separated