反应详情

Thionyl chloride (1 mL) was added dropwise to an ice-cooled solution of 1-(2-hydroxyethyl)-4-(2-fluorophenyl)piperazine (300 mg) and pyridine (1 mL) in benzene (20 mL). After 30 minutes the solution was brought to room temperature and then the flask was immersed in a 60° C. oil bath for 1 hour. The layers were separated and the aqueous fraction was extracted with ethyl acetate (2×20 mL). The combined organic fractions were dried over sodium sulfate and the solvent was removed in vacuo, giving the desired product as a yellow solid (58.6 mg, 18%). ESI-MS m/z 243 (MH+).

1. customwas immersed in a 60° C.
2. customfor 1 hour
3. customThe layers were separated
4. extractionthe aqueous fraction was extracted with ethyl acetate (2×20 mL)
5. dry with materialThe combined organic fractions were dried over sodium sulfate
6. customthe solvent was removed in vacuo