反应详情

温度

-78 °C

A 250 mL round-bottomed flask was charged with 2-(4-(2-((benzyloxy)methyl)-4-(2-thiophenylsulfonyl)-1-piperazinyl)phenyl)-1,1,1-trifluoro-2-propanol (2.93 g, 5.43 mmol) and CH2Cl2 (50 mL) and cooled to −78° C. A 1.0 M solution of BCl3 (1M in CH2Cl2, 7.31 mL, 7.31 mmol, Sigma-Aldrich, St. Louis, Mo.) was added slowly to the mixture and the reaction was stirred for 1 h at −78° C. After this time, MeOH (25 mL) was added and the mixture was warmed to room temperature. After the MeOH was removed in vacuo, diethyl ether (100 mL) was added. The resulting precipitate was collected by filtration, dried under reduced pressure to yield 1,1,1-trifluoro-2-(4-(2-(hydroxymethyl)-4-(2-thiophenylsulfonyl)-1-piperazinyl)phenyl)-2-propanol (2.17 g) as a mixture of four isomers.

1. temperaturethe mixture was warmed to room temperature
2. customAfter the MeOH was removed in vacuo, diethyl ether (100 mL)
3. additionwas added
4. filtrationThe resulting precipitate was collected by filtration
5. customdried under reduced pressure