HRID1018172

反应详情

EQUATION

反应方程式

HRID 1018172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 6.20 ml of an ice-cooled 20% solution of phosgene in toluene was slowly added a solution of 3 g 4-hydroxy-undecanoic acid hex-3-enyl ester and 0.93 g pyridine in 3 ml toluene. The reaction mixture was stirred for 16 hours at room temperature. A mixture of 3.48 g didecylamine and 0.93 g pyridine was added and the mixture was stirred for another 16 hours. Water was added and the mixture extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate, 2N hydrochloric acid, water, dried over magnesium sulfate and evaporated to dryness. The residue was chromatographed on silica gel to give 2.9 g of a colorless liquid.

WORKUP

后处理

  1. additionwas added
  2. stirringthe mixture was stirred for another 16 hours
  3. extractionthe mixture extracted with ethyl acetate
  4. washThe organic layer was washed with saturated sodium bicarbonate, 2N hydrochloric acid, water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness
  7. customThe residue was chromatographed on silica gel