6-Methoxy-1-Indanone → 2-Bromo-6-methoxy-1-indanone

HRID 1107418ノート

反応式

HRID 1107418 の反応式
[Br-:1].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.[CH3:55][O:56][C:57]1[CH:65]=[C:64]2[C:60]([CH2:61][CH2:62][C:63]2=[O:66])=[CH:59][CH:58]=1>CO.ClCCl>[Br:1][CH:62]1[CH2:61][C:60]2[C:64](=[CH:65][C:57]([O:56][CH3:55])=[CH:58][CH:59]=2)[C:63]1=[O:66]

参加物

5

反応物 2

HCID 3340366-Methoxy-1-IndanoneHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 110967482-Bromo-6-methoxy-1-indanone

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

49.2 g (102 mmol) of tetra-n-butylammonium tribromide are added in fractions over the course of 15 minutes, at room temperature, to 16.2 g (100 mmol) of 6-methoxy-indan-1-one dissolved in 400 ml of methanol and 1 litre of dichloromethane, and the mixture is then stirred overnight at room temperature. After evaporation, the residue is taken up in 500 ml of dichloromethane and washed twice with 250 ml of N hydrochloric acid. Drying over magnesium sulphate and concentration, and then rapid filtration over 500 g of silica (eluant:dichloromethane) yield 23.4 g of the desired product.

後処理

  1. customAfter evaporation
  2. washwashed twice with 250 ml of N hydrochloric acid
  3. dry with materialDrying over magnesium sulphate and concentration
  4. filtrationrapid filtration over 500 g of silica (eluant:dichloromethane) yield 23.4 g of the desired product

出典と根拠

ORDレコード
ord-054e6b1ca4804991a8d0d44ba4a7deae
出典データセット
uspto-grants-2000_05
特許番号
US06060487

反応ノート

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