反应详情

To a mixture of (2-amino-5-chlorophenyl)methanol (4.30 g, 27.3 mmol) in dichloromethane (220 ml) was added 2-bromoacetyl bromide (6.06 g, 2.61 ml, 30.0 mmol) at 0-5° C. Stirring for 5 minutes was followed by dropwise addition of aqueous 2 M sodium carbonate solution (130 ml) in approx. 10 minutes. The cooling bath was removed and stirring was continued for 2 h. The solvent was concentrated in vacuo. The aqueous residue was extracted with three 100 ml-portions of ethyl acetate. The combined organic layers were washed with one 50 ml-portion of brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound (7.30 g, 96%) as light grey solid which was used in the next step without purification. MS m/e: 276 ([M+1-1]+).

1. customThe cooling bath was removed
2. stirringstirring
3. waitwas continued for 2 h
4. concentrationThe solvent was concentrated in vacuo
5. extractionThe aqueous residue was extracted with three 100 ml-portions of ethyl acetate
6. washThe combined organic layers were washed with one 50 ml-portion of brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated in vacuo