HRID1197380

反应详情

EQUATION

反应方程式

HRID 1197380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 ml of ethanol was put in a 1-liter four-necked flask, 7.6 g of metal sodium cut into pieces was put therein portionwise to prepare sodium ethoxide. To this were added dropwise 54.6 g of diethyl malonate and then 63.9 g of octyl bromide. Thereafter, the mixture was refluxed for 3 hours. Then, the most part of ethanol was distilled away under the atmospheric pressure, 200 ml of water was added, and the mixture was extracted with 250 ml of ether. The ether solution was dried over sodium sulfate, ether was distilled away, and the residue was distilled under reduced pressure to give 72.1 g of a colorless oily substance (b.p. 111° C./2 mmHg). Yield 85%.

WORKUP

后处理

  1. temperatureThereafter, the mixture was refluxed for 3 hours
  2. distillationThen, the most part of ethanol was distilled away under the atmospheric pressure, 200 ml of water
  3. additionwas added
  4. extractionthe mixture was extracted with 250 ml of ether
  5. dry with materialThe ether solution was dried over sodium sulfate, ether
  6. distillationwas distilled away
  7. distillationthe residue was distilled under reduced pressure
  8. customto give 72.1 g of a colorless oily substance (b.p. 111° C./2 mmHg)