Реакция #1687625

ord-7c7334baa6f44cf3965b5522ee0b1242

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe ether phase was separated
  2. 2
    Экстракцияthe aqueous phase extracted with 3×100 ml of ether
  3. 3
    СушкаThe combined organic phases were dried over magnesium sulphate
  4. 4
    ДругоеRemoval of the solvent in vacuo
  5. 5
    Другоеgave a colorless solid, 66

Методика

A solution of 20 g (0.100 mol) of 65 and 7.5 g (0.150 mol) of potassium hydroxide in 100 ml of water was mixed with a solution of 10 ml (0.160 mol) of methyl iodide in 100 ml of ether. After addition of 1 g of tetrabutylammonium hydrogen sulphate the mixture was stirred overnight at room temperature. The ether phase was separated and the aqueous phase extracted with 3×100 ml of ether. The combined organic phases were dried over magnesium sulphate. Removal of the solvent in vacuo gave a colorless solid, 66. Yield: 17.0 g (0.089 mol, 89%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE036374uspto-grants-1999_11