2-Methoxyphenethyl alcohol → 2-(5-Bromo-2-methoxyphenyl)ethan-1-ol

HRID 264916

반응식

HRID 264916 반응식
[Br-:1].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.[OH:55][CH2:56][CH2:57][C:58]1[CH:63]=[CH:62][CH:61]=[CH:60][C:59]=1[O:64][CH3:65]>ClCCl.CO>[Br:1][C:62]1[CH:61]=[CH:60][C:59]([O:64][CH3:65])=[C:58]([CH2:57][CH2:56][OH:55])[CH:63]=1

참가 물질

5

반응물 2

HCID 819092-Methoxyphenethyl alcoholHCID 23500184Tetra-n-butylammonium tribromide

생성물 1

HCID 15020172-(5-Bromo-2-methoxyphenyl)ethan-1-ol

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

35.72 g of tetrabutylammonium tribromide are added in portions to a solution of 10.7 g of 2-(2-hydroxyethyl)-anisole in 195 ml of dichloromethane and 130 ml of methanol. The reaction mixture is stirred for 150 minutes at room temperature and is then concentrated by evaporation in a rotary evaporator. The residue is partitioned between diethyl ether and water. The organic phases are combined, dried over magnesium sulfate and concentrated by evaporation, and the residue is purified by means of FC (dichloromethane), yielding the title compound: Rf (dichloromethane)=0.26; HPLC Rt =13.04 minutes.

후처리

  1. concentrationis then concentrated by evaporation in a rotary evaporator
  2. customThe residue is partitioned between diethyl ether and water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated by evaporation
  5. customthe residue is purified by means of FC (dichloromethane)

출처 및 근거

ORD 기록
ord-73fe6bf9dfdd47c4b24a39ac196b7dd3
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646143

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