Реакция #346384

ord-aabaacf4c0ca4cecb661f0d684be0442

Уравнение реакции

O
water
CCCOCC(O)CCl
1-chloro-2-hydroxy-3-propoxypropane
O
water
O=S(=O)(O)O
sulphuric acid
O
water
CCCOCC(=O)CCl
1-chloro-3-propoxyacetone
Выход 94.7%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеprepared
  2. 2
    Другоеat 20° C
  3. 3
    workup.ADDITIONwas added
  4. 4
    ЭкстракцияThe mixture was extracted three times with diethyl ether
  5. 5
    Сушкаthe ether extracts dried over sodium sulphate
  6. 6
    Концентрированиеconcentrated under reduced pressure
  7. 7
    Другоеredried

Методика

8N Jones'reagent [30 ml.; prepared by mixing chromium trioxide (8.0 g.), water (15 ml.) and concentrated sulphuric acid (7.5 ml.) and then dilution with water to 30 ml. volume] was added dropwise to a stirred solution of 1-chloro-2-hydroxy-3-propoxypropane (9.1 g.) in acetone (30 ml.) over a period of 30 minutes, keeping the reaction temperature at 20° C. The mixture was then stirred for 4 hours, and then sufficient water to dissolve the precipitated chromium salts was added. The mixture was extracted three times with diethyl ether and the ether extracts dried over sodium sulphate, concentrated under reduced pressure, redried, and reconcentrated to give crude 1-chloro-3-propoxyacetone (8.5 g.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04036872uspto-grants-1977_07