Benzyl Chloride → 3-Iodobenzyloxybenzene

HRID 653585

反応式

HRID 653585 の反応式
[H-].[Na+].[I:3][C:4]1[CH:5]=[C:6]([OH:10])[CH:7]=[CH:8][CH:9]=1.[CH2:11](Cl)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CN(C)C=O.O>[CH2:11]([O:10][C:6]1[CH:5]=[C:4]([I:3])[CH:9]=[CH:8][CH:7]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

6

反応物 3

HCID 7503Benzyl ChlorideHCID 122723-IodophenolHCID 24758Sodium hydride

生成物 1

HCID 42280193-Iodobenzyloxybenzene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

To a suspension of 60% sodium hydride (20 g, 0.5 mol) in dimethylformamide (300 ml), a solution of m-iodophenol (100 g, 0.454 mol}in dimethylformamide was added dropwise and then stirring was continued for 30 min at 70°±5° C. To this reaction mixture, benzyl chloride (57.4 g, 0.454 mol) was added dropwise and the reaction was continued for 2 hours at 100°±5° C. The resultant mixture was taken up in H2O (1l) and extracted with ethyl acetate. The organic extract was washed with H2O, dried over anhydrous MgSO4 and then evaporated. The residual solid was recrystallized from ethanol to give the title compound as white crystals; yield: 119.7 g; mp. 51.0°-53.0° C.

後処理

  1. waitthe reaction was continued for 2 hours at 100°±5° C
  2. extractionextracted with ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with H2O
  5. dry with materialdried over anhydrous MgSO4
  6. customevaporated
  7. customThe residual solid was recrystallized from ethanol

出典と根拠

ORDレコード
ord-65c66d89f2eb4c42baa20ab3eb583ed5
出典データセット
uspto-grants-1992_07
特許番号
US05128062

関連ノート

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