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

HRID 1107418노트

반응식

HRID 1107418 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-054e6b1ca4804991a8d0d44ba4a7deae
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06060487

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