HRID989991

反应详情

EQUATION

反应方程式

HRID 989991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of glycerol (30 g, 326 mmol) and pyridine (25 ml) dissolved in DMF (300 ml) was added dropwise stearoyl chloride (10 g, 33 mmol) dissolved in DMF 100 ml9. The mixture was cooled on an ice bath until addition was complete, whereupon the reaction was maintained under an N2 atmosphere overnight. After 15 hours CH2CL2 (300 ml) and saturated NaHCO3 (aq) was added. The phases were separated and the organic phase washed with water (50 ml) and dried with Na2SO4. The solvent and any pyridine were evaporated under vacuum. The crude product was chromatographed on a silica column (CH2Cl2-MeOH, 20:1) and recrystallised (CH2Cl2-ether) to yield around 7 grams.

WORKUP

后处理

  1. temperatureThe mixture was cooled on an ice bath until addition
  2. temperaturewas maintained under an N2 atmosphere overnight
  3. customThe phases were separated
  4. washthe organic phase washed with water (50 ml)
  5. dry with materialdried with Na2SO4
  6. customThe solvent and any pyridine were evaporated under vacuum
  7. customThe crude product was chromatographed on a silica column (CH2Cl2-MeOH, 20:1)
  8. customrecrystallised (CH2Cl2-ether)
  9. customto yield around 7 grams