反应详情

A mixture of trans-2-(6-fluoro-pyridin-2yl)-cyclopropanecarboxylic acid (˜0.9 mmol) in thionyl chloride (2 mL) was heated at reflux for overnight. The mixture was concentrated and dried under high vacuum for 2 h. Then the residue was dissolved in DCM (4 mL) and added dropwise to a solution of {1-[(4-Bromo-phenylamino)-methyl]-cyclopentyl}-carbamic acid tert-butyl ester (370 mg, 1 mmol) and triethyl amine (280 uL) in DCM (4 mL). The resulting mixture was stirred at rt for over night. The reaction mixture was subjected to flash column directly (20% EtOAc in hexane) to give the desired product as a white solid (348 mg, ˜70%). MS (MH+ 532 and 534).

1. temperaturewas heated
2. temperatureat reflux for overnight
3. concentrationThe mixture was concentrated
4. customdried under high vacuum for 2 h
5. dissolutionThen the residue was dissolved in DCM (4 mL)