Реакция #572012

ord-327f8647fe954b34bbd87b90997492fc

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеby Grignard reaction
  2. 2
    Температураwhile maintaining a temperature of not more than 20° C
  3. 3
    Другоеthe diethyl ether layer was separated from an aqueous layer
  4. 4
    ПромывкаThe ether layer was washed with an aqueous sodium bicarbonate solution
  5. 5
    Промывкаwashed with water
  6. 6
    Сушкаdried over anhydrous sodium sulfate
  7. 7
    Другоеcondensed under reduced pressure

Методика

24.9 g of methyl iodide was reacted with 7.26 g of magnesium in 150 ml of anhydrous diethyl ether to obtain methylmagnesium iodide by Grignard reaction. To a solution consisting of 20 g of 3-phenoxypropionaldehyde and 200 ml of anhydrous diethyl ether was added dropwise the methylmagnesium while maintaining a temperature of not more than 20° C. The reaction solution was added with 25 ml of concentrated hydrochloric acid, and then the diethyl ether layer was separated from an aqueous layer. The ether layer was washed with an aqueous sodium bicarbonate solution, washed with water, dried over anhydrous sodium sulfate and then condensed under reduced pressure to obtain 15.0 g of 4-phenoxy-2-butanol having a boiling point of 61° C. to 62° C. at 3 mmHg in a yield of 67%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04533731uspto-grants-1985_08