Methanol → 1-(Bromomethyl)-2-methoxybenzene

HRID 482481

반응식

HRID 482481 반응식
O[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH3:10].P(Br)(Br)[Br:12].CO.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[Br:12][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH3:10]

참가 물질

6

반응물 4

HCID 887MethanolHCID 10340Sodium CarbonateHCID 24614Phosphorus tribromideHCID 691542-Methoxybenzyl alcohol

생성물 1

HCID 403081-(Bromomethyl)-2-methoxybenzene수율 137.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-hydroxymethyl-2-methoxy-benzene (28.7 gram, 0.207 mol) in CH2Cl2 (574 ml) at 0° C. under nitrogen was added slowly PBr3 (13.66 ml, 0.145 mol). After stirring for an additional 1.5 hours, MeOH (13.66 ml) was added and stirred for 5 minutes. To this mixture was added dropwise 10% Na2CO3 (2 ml) solution and stirred for 5 minutes. The mixture was then washed with 10% Na2 CO3 (50 ml, 2×) and brine (100 ml). It was dried over MgSO4, and filtered. The filtrate was removed under vacuum to give an oil (40 gram) of 1-bromomethyl-2-methoxy-benzene. This material was used without purification.

후처리

  1. stirringstirred for 5 minutes
  2. stirringstirred for 5 minutes
  3. washThe mixture was then washed with 10% Na2 CO3 (50 ml, 2×) and brine (100 ml)
  4. dry with materialIt was dried over MgSO4
  5. filtrationfiltered
  6. customThe filtrate was removed under vacuum

출처 및 근거

ORD 기록
ord-ccfe9963891d4bbe9bb12cfe4029d701
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05798359

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