HRID55454

反应详情

EQUATION

反应方程式

HRID 55454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

137.76 g of (R)-2-hydroxy-3-methoxycarbonyl-2-penten-4-olide are dissolved in 660 ml of toluene and at -10° C. 110 g of methanesulphonyl chloride and then, within a period of 1 hour, 97 g of triethylamine, are added. 350 ml of water and 150 ml of saturated sodium chloride solution are added, the toluene product phase is removed and the aqueous phase is re-extracted twice with 250 ml of toluene. The toluene phases are washed with sodium chloride solution and with water and concentrated by evaporation. Orange-red oil, [α]D20 =+10.6° (3% in CHCl3).

WORKUP

后处理

  1. customthe toluene product phase is removed
  2. extractionthe aqueous phase is re-extracted twice with 250 ml of toluene
  3. washThe toluene phases are washed with sodium chloride solution and with water
  4. concentrationconcentrated by evaporation
  5. customOrange-red oil, [α]D20 =+10.6° (3% in CHCl3)