HRID851413

反应详情

EQUATION

反应方程式

HRID 851413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (6R,7R)-2,2-dimethyl-7-isocyano-1-aza-3-oxabicyclo[4.2.0]octan-8-one (150 mg), tribulyltinhydride (0.263 ml), and azobisisobutyronitrile (14 mg) in benzene (4.5 ml) was refluxed for 15 minutes. The resulting solution was chromatographed on silica gel (4.5 g) eluting with a mixture of benzene and acetone (15:1-6:1) to give the crude product (140 mg) as an oil, which was purified by silica gel (5 g) chromatography (eluate: a mixture of methylene chloride and ethyl acetate 30:1-5:1) to give (6R)-2,2-dimethyl-1-aza-3-oxabicycle[4.2.0]octan-8-one (98 mg) as an oil.

WORKUP

后处理

  1. temperaturewas refluxed for 15 minutes
  2. customThe resulting solution was chromatographed on silica gel (4.5 g)
  3. washeluting with a mixture of benzene and acetone (15:1-6:1)
  4. customto give the crude product (140 mg) as an oil, which
  5. customwas purified by silica gel (5 g) chromatography (eluate
  6. additiona mixture of methylene chloride and ethyl acetate 30:1-5:1)