HRID10761

反应详情

EQUATION

反应方程式

HRID 10761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7.50 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 25 ml of methanol, 2 ml of water and 1.0 ml of concd. hydrochloric acid was stirred at 30° C. for 1 h. The reaction mixture was concentrated to a volume of 10 ml and after adding 50 ml of water the pH of the hot solution was adjusted to 8 with 10% aqueous sodium hydroxide. After cooling the precipitated crystals were filtered off, and dried at 40° C. until the weight was constant to yield 6.06 g (93.5%) of the title compound. M.p.: 139–140° C.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to a volume of 10 ml
  2. additionafter adding 50 ml of water the pH of the hot solution
  3. temperatureAfter cooling the precipitated crystals
  4. filtrationwere filtered off
  5. customdried at 40° C. until the weight