2-Ethyl-1-butanol → 4-Bromomethyl-benzoic acid 2-ethyl-butyl ester

HRID 1591983ノート

反応式

HRID 1591983 の反応式
[Br:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.[CH2:12]([CH:14]([CH2:17][CH3:18])[CH2:15][OH:16])[CH3:13]>C(Cl)Cl>[CH2:12]([CH:14]([CH2:17][CH3:18])[CH2:15][O:16][C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:3]([CH2:2][Br:1])=[CH:4][CH:5]=1)[CH3:13]

参加物

4

反応物 2

HCID 73582-Ethyl-1-butanolHCID 50682894-Bromomethyl-benzoyl chloride

生成物 1

HCID 671383384-Bromomethyl-benzoic acid 2-ethyl-butyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of the title A compound, 4-bromomethyl-benzoyl chloride (466 mg, 2 mmol) in 3 mL of CH2Cl2 is added dropwise to a solution of 2-ethyl-1-butanol (204 mg, 2 mmol) and TEA (202 mg, 2 mmol) in 10 mL of CH2Cl2 at 0˜5° C. over 30 min. The reaction is allowed to warm to RT and stirred overnight. The solvent is evaporated and the residue is partitioned between hexane and water. The organic phase is dried over anhydrous MgSO4 and concentrated. The residue is chromatographic on silica gel using EtOAc/hexane (gradient 90-70) to give 4-bromomethyl-benzoic acid 2-ethyl-butyl ester as a colorless oil.

後処理

  1. customThe solvent is evaporated
  2. customthe residue is partitioned between hexane and water
  3. dry with materialThe organic phase is dried over anhydrous MgSO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-e165bb54b2b742f79303a7e3dbe9fbff
出典データセット
uspto-grants-2007_11
特許番号
US07291635B2

反応ノート

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