反应详情

Solid 5-bromo-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 5, method C; 200 mg, 0.651 mmol) was added to a stirred suspension of CDI (106 mg, 0.651 mmol) in THF (10 ml) under nitrogen at 20° C. The reaction mixture was stirred at room temperature for 10 min and 4-pyridazinamine (may be prepared as described in Description 11; 61.9 mg, 0.65 mmol) was added dropwise. After refluxing for 14 h, the reaction mixture was concentrated. Water was added to the residue and the mixture was extracted with ethyl acetate (3×50 ml). The organic phase was washed with saturated brine (25 ml), dried over sodium sulphate and evaporated in vacuo. The residue was washed with methanol to yield the title compound as a white solid. 95 mg.

1. temperatureAfter refluxing for 14 h
2. concentrationthe reaction mixture was concentrated
3. additionWater was added to the residue
4. extractionthe mixture was extracted with ethyl acetate (3×50 ml)
5. washThe organic phase was washed with saturated brine (25 ml)
6. dry with materialdried over sodium sulphate
7. customevaporated in vacuo
8. washThe residue was washed with methanol