反应详情

A solution of ethyl 2-(2,2-dichlorocyclopropyloxy- imino)-3,3-ethylenedioxybutyrate (syn isomer)(312 mg) and tri-n-butyltinhydride (0.55 ml) in toluene (2 ml) was refluxed under nitrogen atmosphere in the presence of catalytic amount of 2,2-azobisisobutyronitrile for hours. The reaction mixture was concentrated in vacuo. The residue was subjected to column chromatography on silica gel (24 g) and eluted with a mixture of diethyl ether and n-hexane (1:2 V/V). The fractions containing the compound, which had higher Rf-value on TLC [development solvent system:diethyl ether and n-hexane (2:1 V/V)], were collected and concentrated in vacuo to give ethyl 2-(2-chlorocyclopropyloxyimino)-3,3-ethylenedioxybutyrate (syn isomer)(94 mg).

1. concentrationThe reaction mixture was concentrated in vacuo
2. washeluted with a mixture of diethyl ether and n-hexane (1:2 V/V)
3. additionThe fractions containing the compound, which
4. customwere collected
5. concentrationconcentrated in vacuo