反应详情

温度

20 °C

3-Pyridinamine (123 mg, 1.30 mmol) in DCM (15 ml) was added to a stirred solution of 5-bromo-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 5, method A; 200 mg, 0.65 mmol), HOBT (150 mg, 0.98 mmol) and EDC (187 mg, 0.98 mmol) in DCM (15 ml) under nitrogen at room temperature. The reaction mixture was stirred at 20° C. overnight. The reaction mixture was partitioned between DCM (50 ml) and water (25 ml). The organic phase was washed with saturated brine (25 ml), dried over sodium sulphate and evaporated in vacuo to give the crude product as a yellow solid. The crude product was added to a Biotage column and was eluted with petroleum ether:ethyl acetate (3:1) to yield the title compound as a white solid. 75 mg. MS (electrospray): m/z [M+H]+=383

1. customThe reaction mixture was partitioned between DCM (50 ml) and water (25 ml)
2. washThe organic phase was washed with saturated brine (25 ml)
3. dry with materialdried over sodium sulphate
4. customevaporated in vacuo
5. customto give the crude product as a yellow solid
6. washwas eluted with petroleum ether:ethyl acetate (3:1)