HRID1857049

反应详情

EQUATION

反应方程式

HRID 1857049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

50 g (120 mmol; 1 eq.) of 6-O-palmitoyl-L-ascorbic acid were dissolved in 400 ml of pyridine in a 1 l 4-necked flask. 23.40 g (130 mmol; 1.1 eq.) of sorboyl chloride, dissolved in 30 ml of dichloromethane, were slowly added dropwise at an internal temperature of -15° C. Care was taken here that the internal temperature did not exceed -10° C. The mixture was brought to room temperature and additionally stirred for 2 hours. The reaction solution was concentrated on a rotary evaporator and then codistilled with toluene. The residue was taken up in a little dichloromethane and extracted with 1 M HCl. The organic phase was concentrated somewhat and treated with an excess of n-hexane. A white precipitate was deposited, which was dried in an oil pump vacuum.

WORKUP

后处理

  1. additionwere slowly added dropwise at an internal temperature of -15° C
  2. customdid not exceed -10° C
  3. customwas brought to room temperature
  4. concentrationThe reaction solution was concentrated on a rotary evaporator
  5. extractionextracted with 1 M HCl
  6. concentrationThe organic phase was concentrated somewhat
  7. additiontreated with an excess of n-hexane
  8. customwhich was dried in an oil pump vacuum