反应详情

To a solution of 5-benzyloxy-2-[1-(4-chlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid cyclopropylmethyl-(2-hydroxyethyl)-amide (330) (390 mg, 0.73 mmol) in dichloromethane (30 mL) was added triphenyl phosphine (286 mg, 1.09 mmol) and diisopropyl azodicarboxylate (0.22 mL, 1.09 mmol) at room temperature the reaction was stirred for 30 minutes (TLC; 5% methanol in ethyl acetate/UV/SiO2, Rf=0.05). The dichloromethane was removed in vacuo and the crude mass was purified by silica gel (normal, 100-200 mesh) column chromatography using gradient eluent of 1% to 5% methanol in dichloromethane to get pure 9-benzyloxy-6-[1-(4-chlorophenyl)-cyclopentylmethyl]-2-cyclopropylmethyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (331) (280 mg, 74%) as a white sticky solid.

1. customThe dichloromethane was removed in vacuo
2. customthe crude mass was purified by silica gel (normal, 100-200 mesh) column chromatography