Реакция #309663

Уравнение реакции

indane

Methacryloyl chloride

AlCl3

HCl

→

2-methyl-3,5,6,7-tetrahydro-s-indacen-1(2H)-one

Растворители

CH2Cl2

Условия реакции

Обработка

1. 1
   workup.STIRRINGwas stirred overnight
2. 2
   ДругоеNext day the mixture obtained
3. 3
   ДругоеThe organic phase was separated
4. 4
   Промывкаwashed by water, 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 suspension of 133.5 r AlCl3 (1 mol) in 500 ml CH2Cl2 at −78° C., stirred 20 min. Then indane (59 g, 0.5 mol) was added at the same temperature, allowed to warm to room temperature and then was stirred overnight. Next day the mixture obtained was poured carefully into mixture of ice (1000 g) and HCl (200 ml). The organic phase was separated, washed by water, 5% NaHCO3, and dried over MgSO4. Solvent was evaporated and residue was distilled in vacuum given 77.6 of product (83%), b.p. 118-120° C./0.5 torr.

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