反应详情

1.39 g (0.0367 mol) of sodium borohydride in 30 ml of water were slowly added dropwise to a mixture of 16.2 g (0.05 mol) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one (prepared as described in Example 1) and 3.86 g (0.035 mol) of calcium chloride in 250 ml of isopropanol at -15° C. After 18 hours, the reaction mixture was concentrated in vacuo, the residue was taken up in methylene chloride, and the solution was washed with water, dried over sodium sulphate, filtered, and concentrated again. The oily residue crystallized after being triturated with diisopropyl ether. 14.3 g (87% of theory) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl) -pentan-3-ol of melting point 84° C. were obtained.

1. concentrationthe reaction mixture was concentrated in vacuo
2. washthe solution was washed with water
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated again
6. customThe oily residue crystallized
7. customafter being triturated with diisopropyl ether