反应详情

温度

130 °C

A solution of tert-butyl N-allyl-N-[-2-hydroxyimino-2-phenyl-ethyl]carbamate as a mixture of E and Z isomers (3.2 g, 10.9 mmol) in xylene (100 mL) is stirred at 100° C. for 2 hours, 130° C. for 6 hours, 100° C. for 12 hours and 130° C. for 2 hours. The cooled reaction is concentrated under reduced pressure to give a residue. The residue is purified by silica gel flash chromatography, eluting with hexane/ethyl acetate (1:0) to hexane/ethyl acetate (0:1) to give the title compound (1.5 g, 48%). ES/MS (m/e): 291 (M+H).

1. customThe cooled reaction
2. concentrationis concentrated under reduced pressure
3. customto give a residue
4. customThe residue is purified by silica gel flash chromatography
5. washeluting with hexane/ethyl acetate (1:0) to hexane/ethyl acetate (0:1)