Benzyl Chloride → 3-Iodobenzyloxybenzene

HRID 653585

반응식

HRID 653585 반응식
[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

참가 물질

6

반응물 3

HCID 7503Benzyl ChlorideHCID 122723-IodophenolHCID 24758Sodium hydride

생성물 1

HCID 42280193-Iodobenzyloxybenzene

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-65c66d89f2eb4c42baa20ab3eb583ed5
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05128062

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