HRID1719318
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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), tributyltinhydride (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 (15:1-16:1) 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
- temperaturewas refluxed for 15 minutes
- customThe resulting solution was chromatographed on silica gel (4.5 g)
- washeluting with a mixture of benzene and acetone (15:1-16:1)
- customto give the crude product (140 mg) as an oil, which
- customwas purified by silica gel (5 g) chromatography (eluate
- additiona mixture of methylene chloride and ethyl acetate 30:1-5:1)