HRID1420764

反应详情

EQUATION

反应方程式

HRID 1420764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

(3S,4S)-6-(3-tert-butyldimethylsilyloxyphenyl)sulphonyl-3,4-dihydro-3,4-epoxy-2,2,3-trimethyl-2H-benzo[b]pyran (2.2 g) (see Preparation 15) was dissolved in ethanol (25 ml) and 35% aqueous ammonia solution (25 ml) was added. The mixture was heated at 40-50° C. for 24 hours. The solvent was removed under reduced pressure and the residue was chromatographed on silica using 7.5:92.5 methanol:dichloromethane as the eluent to yield (3S,4R)-4-amino-3,4-dihydro-3-hydroxy-6-(3-hydroxyphenyl)sulphonyl-2,2,3-trimethyl-2H-benzo[b]pyran (1.42 g) as a foam. Found: C,54.39; H,5.22; N,3.19. C18H21NO5S, 0.50 CH2Cl2 requires C,54.75; H,5.46; N,3.45%.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was chromatographed on silica using 7.5:92.5 methanol