Lithium Bromide → 1-(2-Bromo-ethoxymethyl)-4-chlorobenzene

HRID 2261246노트

반응식

HRID 2261246 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][O:7][CH2:8][CH2:9]OS(C)(=O)=O)=[CH:4][CH:3]=1.[Br-:17].[Li+]>CC(C)=O>[Br:17][CH2:9][CH2:8][O:7][CH2:6][C:5]1[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=1

참가 물질

4

실험 절차

A mixture of methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester (Intermediate 6) (1.37 g, 5.18 mmol) and lithium bromide (1.80 g, 20.7 mmol) in acetone (15 mL) was heated at reflux overnight. The reaction mixture was concentrated to dryness and the residue partitioned between DCM and water. The organic layer was dried (MgSO4), and concentrated, and purified by column chromatography over silica using DCM/cyclohexane (1:3) as eluent to afford the product as a colourless oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. concentrationThe reaction mixture was concentrated to dryness
  4. customthe residue partitioned between DCM and water
  5. dry with materialThe organic layer was dried (MgSO4)
  6. concentrationconcentrated
  7. custompurified by column chromatography over silica

출처 및 근거

ORD 기록
ord-59ca3905a1594c12915c5fbac4032272
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07846955B2

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