HRID266070

反应详情

EQUATION

反应方程式

HRID 266070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (±)-4-[4-[4-[4-[[(1,1-dimethylethyl)dimethylsilyl]oxy]phenyl]-1-piperazinyl]phenyl]-2,4-dihydro-2-[2-hydroxy-2-[4-(trifluoromethoxy)phenyl]ethyl]-5-methyl-3H-1,2,4-triazol-3-one (0.0043 mol) was dissolved in dichloromethane (100 ml) upon stirring. A solution of tetrabutylammonium fluoride in tetrahydrofuran (0.0045 mol) was added and the mixture was stirred at room temperature for 15 minutes. Water was added and the mixture was stirred for 30 minutes. The precipitate was filtered off, dried and crystallized from n-butanol, yielding 1.1 g (58.2%) of (±)-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-2-[2-hydroxy-2-[4-(trifluoromethoxy)-phenyl]ethyl]-5-methyl-3H-1,2,4-triazol-3-one; mp. 230.6° C. (comp. 36).

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 15 minutes
  2. stirringthe mixture was stirred for 30 minutes
  3. filtrationThe precipitate was filtered off
  4. customdried
  5. customcrystallized from n-butanol