Реакция #214064

ord-a3246066df934bcdb734d5e1ca7c885a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for a further 15 hours
  2. 2
    Промывкаthe organic phase was washed three times with 100 ml of water each time
  3. 3
    СушкаThe organic phase was dried over sodium sulphate
  4. 4
    workup.DISTILLATIONthe solvent was distilled off under a waterpump vacuum and 100 ml of ether
  5. 5
    workup.ADDITIONwere added to the residue

Методика

25 g (0.08 mol) of 1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-3,3-dimethyl-4-hydroxy-butan-2-one were dissolved in 350 ml of isopropanol, and 3.5 g of sodium borohydride were added in portions at room temperature. The mixture was stirred at room temperature for 15 hours, 500 ml of water were added, the mixture was stirred at room temperature for a further 15 hours, 300 ml of methylene chloride were added and the organic phase was washed three times with 100 ml of water each time. The organic phase was dried over sodium sulphate, the solvent was distilled off under a waterpump vacuum and 100 ml of ether were added to the residue. 17 g (67.6% of theory) of 1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-3,3-dimethyl-butane-2,4-diol were obtained as colorless crystals of melting point 110°-112° C. ##STR19##

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04254132uspto-grants-1981_03