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4-Methoxy-3-(4-methoxy-2-butenyl)-bromobenzene → 4-Bromo-1-methoxy-2-(4-methoxybutyl)benzene

HRID 744853
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반응식

HRID 744853 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([Br:9])=[CH:5][C:4]=1[CH2:10][CH:11]=[CH:12][CH2:13][O:14][CH3:15]>O1CCCC1.[Pt]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([Br:9])=[CH:5][C:4]=1[CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 541427744-Methoxy-3-(4-methoxy-2-butenyl)-bromobenzene

생성물 1

HCID 214586274-Bromo-1-methoxy-2-(4-methoxybutyl)benzene

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 50 g of 4-methoxy-3-(4-methoxy-2-butenyl)-bromobenzene in 700 ml of tetrahydrofuran is hydrogenated for 2 hours under normal pressure and at room temperature in the presence of 2.5 g of 5% Pt/C. The reaction mixture is filtered. The filtrate is concentrated by evaporation. The evaporation residue obtained from the filtrate is purified by FC (1.6 kg of silica gel, hexane/ethyl acetate=20:1). Distillation under a high vacuum yields the title compound: Rt (hexane/ethyl acetate=10:1)=0.38; HPLC Rt =19.92 minutes; FAB-MS (M+H)+ =273.

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후처리

  1. filtrationThe reaction mixture is filtered
  2. concentrationThe filtrate is concentrated by evaporation
  3. customThe evaporation residue obtained from the filtrate
  4. customis purified by FC (1.6 kg of silica gel, hexane/ethyl acetate=20:1)
  5. distillationDistillation under a high vacuum

출처 및 근거

ORD 기록
ord-2df88ef682954b54a4a4e698c87f16a0
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05559111

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