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

HRID 222481

反応式

HRID 222481 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75ec45925fb84254861ee6335275f203
出典データセット
uspto-grants-2012_06
特許番号
US08207269B2

関連ノート

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