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Aluminum(III) Chloride → HCID 22172947、化合物

HRID 716455
ノート
印刷プレビュー

反応式

HRID 716455 の反応式
[Al+3].[Cl-].[Cl-].[Cl-].[Br:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:18])=[C:10]([CH2:12][CH:13]([CH3:17])[C:14](Cl)=[O:15])[CH:11]=1>ClCCl>[Br:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:18])=[C:10]2[C:11]=1[C:14](=[O:15])[CH:13]([CH3:17])[CH2:12]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 89392410HCID 89392410、化合物

生成物 1

HCID 22172947HCID 22172947、化合物収率 99.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred suspension of 49.5 g (0.371 mol, 1.2 eq.) of AlCl3 in 300 ml of dichloromethane a solution of 85.3 g (0.310 mol) of 3-(5-bromo-2-methylphenyl)-2-methylpropanoyl chloride in 50 ml of dichloromethane was added dropwise. This mixture was stirred overnight at room temperature and then poured on 500 g of ice. The organic layer was separated, and the aqueous layer was additionally extracted with 3×75 ml of dichloromethane. The combined organic extract was washed by aqueous K2CO3, dried over K2CO3, passed through a short pad of silica gel, and then evaporated to dryness. This procedure gave 74.0 g (>99%) of 7-bromo-2,4-dimethylindan-1-one as a light-orange liquid, solidified at room temperature, which was further used without an additional purification.

後処理

  1. additionwas added dropwise
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was additionally extracted with 3×75 ml of dichloromethane
  4. extractionThe combined organic extract
  5. washwas washed by aqueous K2CO3
  6. dry with materialdried over K2CO3
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-48aa8145633b4c919197a4210979fdaa
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187583B2

反応ノート

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