Water → 2-Benzyloxy-5-(trifluoromethoxy)benzene

HRID 583027ノート

反応式

HRID 583027 の反応式
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:9][C:10]([F:20])([F:19])[O:11][C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:1]([O:18][C:15]1[CH:16]=[CH:17][C:12]([O:11][C:10]([F:9])([F:19])[F:20])=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenol

生成物 1

HCID 215840942-Benzyloxy-5-(trifluoromethoxy)benzene収率 99%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Benzyl bromide (66.17 ml, 95.35 g, 0.56 mol) was added to a mixture of 4-(trifluoromethoxy)phenol (90.26 g, 0.51 mol) and potassium carbonate (140.97 g, 1.2 mol) in dimethylformamide (160 ml) and the mixture was stirred at room temperature for 72 hours. The mixture was poured into water (1.5 l) and extracted with ethyl acetate (3×500 ml). The combined organic fractions were washed with aqueous sodium carbonate (saturated, 500 ml), dried (MgSO4) and the solvent was evaporated under reduced pressure to give the title compound as a colorless solid (133.5 g, 99%). 1H NMR (360 MHz, CDCl3) δ7.39 (5 H, m), 7.14 (2 H, d, J=9.0 Hz), 6.95 (2 H, d, J=9.0 Hz), and 5.05 (2 H, s).

後処理

  1. extractionextracted with ethyl acetate (3×500 ml)
  2. washThe combined organic fractions were washed with aqueous sodium carbonate (saturated, 500 ml)
  3. dry with materialdried (MgSO4)
  4. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-553d9c3dca1d457bab9d43a075482098
出典データセット
uspto-grants-1999_07
特許番号
US05929054

反応ノート

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