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

HRID 2261246ノート

反応式

HRID 2261246 の反応式
[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

参加物

4

反応物 2

HCID 82050Lithium BromideHCID 59593471Methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester2 回

生成物 1

HCID 136543741-(2-Bromo-ethoxymethyl)-4-chlorobenzene

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59ca3905a1594c12915c5fbac4032272
出典データセット
uspto-grants-2010_12
特許番号
US07846955B2

反応ノート

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