反应详情

A solution of 50.0 g (195 mmol) of N-(4-bromophenyl)-3-oxobutyramide in 217 mL of concentrated sulfuric acid was heated to 120° C. for 1 hour. After cooling to RT, the reaction solution was added to 1.5 L of ice water, stirred for 30 minutes, and the precipitate formed was filtered and washed with 4 L of water. Subsequently it was dried at 35° C. in the circulating air dryer until a constant weight was achieved. Yield: 24.0 g (52% of theoretical); C10H8BrNO (M=238.081); calc.: molpeak (M+H)+: 238/240 (Br); found: molpeak (M+H)+: 238/240 (Br); HPLC-MS: 4.8 minutes (method B).

1. customthe precipitate formed
2. filtrationwas filtered
3. washwashed with 4 L of water
4. customSubsequently it was dried at 35° C. in the circulating air dryer until a constant weight
5. custom4.8 minutes (method B)