Hydrochloric Acid → 3,5,6,7-Tetrahydro-2-methyl-s-indacen-1(2H)-one

HRID 222481

반응식

HRID 222481 반응식
[C:1](Cl)(=[O:5])[C:2]([CH3:4])=[CH2:3].[Al+3].[Cl-].[Cl-].[Cl-].[CH2:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:13][CH2:12]1.Cl>C(Cl)Cl>[CH3:3][CH:2]1[CH2:4][C:17]2[C:16](=[CH:15][C:14]3[CH2:13][CH2:12][CH2:11][C:19]=3[CH:18]=2)[C:1]1=[O:5]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 10326IndaneHCID 13528Methacryloyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 109542593,5,6,7-Tetrahydro-2-methyl-s-indacen-1(2H)-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  1. stirringwas stirred overnight
  2. customNext day the mixture obtained
  3. customThe organic phase was separated
  4. washwashed by water, 5% NaHCO3
  5. dry with materialdried over MgSO4
  6. customSolvent was evaporated
  7. distillationresidue was distilled in vacuum

출처 및 근거

ORD 기록
ord-75ec45925fb84254861ee6335275f203
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207269B2

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