反应详情

The solution of 3,5-dibromobenzoic acid (26 g, 93 mmol) in SOCl2 (100 mL) was heated at reflux for 2 h, concentrated, diluted with dry DCM (300 mL) and added slowly to a stirred solution of N,O-dimethylhydroxylamine hydrochloride (9.75 g, 100 mmol) and EtN3 (28 g, 277 mmol) in dry DCM (300 mL) at 0° C. The solution was stirred for 1 h at rt, poured into water and the organic layer was separated. The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated to give crude compound P37a (28 g, 93%) as an oil.

1. temperatureat reflux for 2 h
2. concentrationconcentrated
3. additiondiluted with dry DCM (300 mL)
4. customthe organic layer was separated
5. washThe organic layer was washed with water and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customto give crude compound P37a (28 g, 93%) as an oil