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

HRID 1452119

반응식

HRID 1452119 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 then concentrated by evaporation using a rotary evaporator. The residue is partioned between diethyl ether and water. The organic phases are combined, dried over magnesium sulfate and concentrated by evaporation and the residue is pudfied by means of FC (dichloromethane) to yield the title compound: Rf (dichloromethane)=0.26; HPLC Rt =13.0 minutes.

후처리

  1. concentrationconcentrated by evaporation
  2. customa rotary evaporator
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-efa0af2f5ba4469aa4fcb0fba124c16d
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606078

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