2-Bromophenol → 1-(Benzyloxy)-2-bromobenzene

HRID 31350

反応式

HRID 31350 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].[CH2:9](Cl)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 72442-BromophenolHCID 7503Benzyl ChlorideHCID 11430Potassium Carbonate

生成物 1

HCID 5618281-(Benzyloxy)-2-bromobenzene収率 94.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 35 g of 1-bromo-2-hydroxy-benzene, 30.5 g of benzyl chloride and 50 g of K2CO3 in 500 ml of acetone is refluxed for 12 hours. The reaction mixture is concentrated under vacuum, the residue is taken up in a water/EtOAc mixture, the organic phase is washed with 1N NaOH solution and with water and dried over Na2SO4, and the solvent is evaporated off under vacuum. The resulting oil is distilled under reduced pressure to give 50.3 g of the expected product, b.p.=155° C. at 40 Pa.

後処理

  1. temperatureis refluxed for 12 hours
  2. concentrationThe reaction mixture is concentrated under vacuum
  3. washthe organic phase is washed with 1N NaOH solution and with water
  4. dry with materialdried over Na2SO4
  5. customthe solvent is evaporated off under vacuum
  6. distillationThe resulting oil is distilled under reduced pressure

出典と根拠

ORDレコード
ord-4bba665bcc164f27aa90061a113de7b7
出典データセット
uspto-grants-2008_09
特許番号
US07425566B2

関連ノート

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