反应详情

温度

70 °C

A mixture of ethyl 2-amino-2-thioxoacetate (50.9 mg, 0.38 mmol) and 3-bromo-1-(3-bromophenyl)butan-2-one (0.38 mmol, crude from previous step) in DMF (2 mL) was stirred at 70° C. for 12 h. The mixture was diluted with EtOAc and washed with H2O. The organic layer was concentrated, and purified by silica gel column chromatography(0-50% EtOAc/Hexane) to yield a yellowish solid (71 mg, 55% over 2 steps). MS (ES+) C14H14BrNO2S requires: 339, 341 found: 340, 342 [M+H]+(1:1).

1. washwashed with H2O
2. concentrationThe organic layer was concentrated
3. custompurified by silica gel column chromatography(0-50% EtOAc/Hexane)
4. customto yield a yellowish solid (71 mg, 55% over 2 steps)