Diethyl Ether → 4-Benzyloxybenzotrifluoride

HRID 269550ノート

反応式

HRID 269550 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][CH:3]=1.[CH2:12](Br)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)C>CC(C)=O.O>[CH2:12]([O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:9])([F:10])[F:11])=[CH:4][CH:3]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 678744-(Trifluoromethyl)phenol

生成物 1

HCID 27981684-Benzyloxybenzotrifluoride

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

A solution of 4-hydroxybenzotrifluoride (8.55 g, 52.78 mmol) in acetone (200 ml) was treated with benzyl bromide (9.87 g, 6.86 ml, 58.05 mmol) and potassium carbonate (10.94 g, 79.16 mmol). The mixture was stirred and heated to reflux under nitrogen for 3 h. After cooling, diethyl ether (400 ml) and water (400 ml) were added and the aqueous phase re-extracted with diethyl ether (100 ml). The combined organic layers were washed with water, dried (MgSO4) and the solvent removed in vacuo to leave the title compound as a white solid. (12.71 g, 95%)

後処理

  1. temperatureheated
  2. temperatureto reflux under nitrogen for 3 h
  3. temperatureAfter cooling
  4. extractionthe aqueous phase re-extracted with diethyl ether (100 ml)
  5. washThe combined organic layers were washed with water
  6. dry with materialdried (MgSO4)
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-81ae0fc634cb473dbd06177920facf11
出典データセット
uspto-grants-2008_11
特許番号
US07446222B2

反応ノート

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