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HCID 13935580, 화합물 → N-(4-benzyloxy-3,3-difluorobutyl)phthalimide

HRID 2309590
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HRID 2309590 반응식
[CH2:1]([O:8][CH2:9][C:10]([F:19])([F:18])[CH2:11][CH2:12]OS(C)(=O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:20]1(=[O:30])[NH:24][C:23](=[O:25])[C:22]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:21]12.[K]>CN(C=O)C>[CH2:1]([O:8][CH2:9][C:10]([F:19])([F:18])[CH2:11][CH2:12][N:24]1[C:23](=[O:25])[C:22]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:21]2[C:20]1=[O:30])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 13935580HCID 13935580, 화합물HCID 24194345Phthalimide potassium salt

생성물 1

HCID 13935581N-(4-benzyloxy-3,3-difluorobutyl)phthalimide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 1-benzyloxy-2,2-difluoro-4-methanesulfonyloxybutane (63.44 g, 0.216 moles), potassium phthalimide (44 g, 0.238 moles) and dry DMF (500 mL), distilled from CaH2) is stirred and heated at 100° C. After a short time the mixture solidifies, and an additional dry DMF (500 mL) is added. Upon heating at 90°-100° C. for another 20 hours, salts are removed by filtration, and the DMF is distilled under vacuum (oil pump). The residue is dissolved in CH2Cl2 (800 mL) and washed with 1N KOH (twice) and 1N HCl (twice). Drying (Na2SO4) and evaporation yields N-(4-benzyloxy-3,3-difluorobutyl)-phthalimide as a yellow oil: 68.5 g (92%).

후처리

  1. distillationdistilled from CaH2)
  2. additionan additional dry DMF (500 mL) is added
  3. temperatureUpon heating at 90°-100° C. for another 20 hours
  4. customsalts are removed by filtration
  5. distillationthe DMF is distilled under vacuum (oil pump)
  6. dissolutionThe residue is dissolved in CH2Cl2 (800 mL)
  7. washwashed with 1N KOH (twice) and 1N HCl (twice)
  8. customDrying
  9. custom(Na2SO4) and evaporation

출처 및 근거

ORD 기록
ord-eaeec1bd7a0143b39af24eb9a3485903
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04695654

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