HRID1165697

反应详情

EQUATION

反应方程式

HRID 1165697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

26 g (0.1 mol) of 1-cyclohexyl-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-one(prepared as described in Example II-1) were taken up in 200 methanol, and 4.5 g of sodium borohydride were added in portions to the solution, while stirring and cooling. After the reaction had ended, the reaction mixture was adjusted to pH 6 and was concentrated. The residue was taken up in 200 ml of methylene chloride, and the solution was washed with saturated sodium bicarbonate solution, dried over sodium sulphate, filtered and concentrated. The residue was recrystallized from petroleum ether. 14.5 g (55% of theory) of 1-cyclohexyl-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-ol of melting point 131° C. were obtained.

WORKUP

后处理

  1. additionwere added in portions to the solution
  2. temperaturecooling
  3. concentrationwas concentrated
  4. washthe solution was washed with saturated sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was recrystallized from petroleum ether