反应详情

温度

110 °C

A mixture of methyl ester from Step 1 (0.28 g, 0.68 mmol) and 4-fluorobenzylamine (0.16 mL, 1.43 mmol) in toluene (5 mL) was heated in an oil bath at 110° C. overnight. The resultant precipitate was filtered, washed with diethyl ether, and dried under vacuum. The solid was dissolved in DMSO and subjected to HPLC purification on C-18 stationary phase eluted with water/acetonitrile/TFA mobile phase. Collection and lyophilization of appropriate fractions provided the title compound as yellow solid.

1. filtrationThe resultant precipitate was filtered
2. washwashed with diethyl ether
3. customdried under vacuum
4. dissolutionThe solid was dissolved in DMSO
5. customsubjected to HPLC purification on C-18 stationary phase
6. washeluted with water/acetonitrile/TFA mobile phase
7. customCollection and lyophilization of appropriate fractions