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

HRID 619105ノート

反応式

HRID 619105 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 liter 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-0d29853eb1df4f9bbbc87be44da6c75a
出典データセット
uspto-grants-1999_09
特許番号
US05958927

反応ノート

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