反应详情

2-Formylheptanonitrile (10.7 g), sodium acetate (7.9 g) and aminoacetonitrile hydrochloride (8.9 g) were mixed together in 200 ml of methanol:water (8:2). After stirring for 2 hours at ambient temperature the methanol was removed under aspirator vacuum and the residue partitioned between ethyl acetate and water. The layers were separated and the ethyl acetate layer was washed with brine, dried (Na2SO4) and concentrated to leave a yellow oil. Chromatographic purification of the material over silica gel using ethyl acetate/hexane as the eluent afforded a light yellow solid as a mixture of isomers (11.6 g, 85%); tlc, Rf =0.37 and 0.50 silica gel, ethyl acetate:hexane (1:1).

1. customwas removed under aspirator vacuum
2. customthe residue partitioned between ethyl acetate and water
3. customThe layers were separated
4. washthe ethyl acetate layer was washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customto leave a yellow oil
8. customChromatographic purification of the material over silica gel
9. customafforded a light yellow solid
10. additionas a mixture of isomers (11.6 g, 85%)