Реакция #975502

ord-2a42855ca1464ae8bf5191ba4049d345

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGwas stirred overnight
  2. 2
    ДругоеNext day the mixture obtained
  3. 3
    ДругоеThe organic phase was separated
  4. 4
    Промывкаwashed with water and 5% NaHCO3
  5. 5
    Сушкаdried over MgSO4
  6. 6
    ДругоеSolvent was evaporated
  7. 7
    workup.DISTILLATIONresidue was distilled in vacuum

Методика

Methacryloyl chloride (50 ml, 0.5 mol) was added to a suspension of 133.5 g (1 mol) AlCl3 in 500 ml CH2Cl2 at −78° C. and stirred for 20 min. Then 59 g (0.5 mol) indane was added at the same temperature. The mixture was allowed to warm to room temperature and then was stirred overnight. Next day the mixture obtained was poured carefully into a mixture of ice (1000 g) and HCl (200 ml). The organic phase was separated, washed with water and 5% NaHCO3, and dried over MgSO4. Solvent was evaporated and residue was distilled in vacuum giving 77.6 g of product (83%), b.p. 118-120° C./0.5 torr.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08247587B2uspto-grants-2012_08