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Chlorotrimethylsilane → N4-(cyclohexyloxycarbonyl)-5'-deoxy-5-fluorocytidine

HRID 2259172
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HRID 2259172 반응식
[F:1][C:2]1[C:3]([NH2:17])=[N:4][C:5](=[O:16])[N:6]([CH:15]=1)[C@@H:7]1[O:14][C@H:12]([CH3:13])[C@@H:10]([OH:11])[C@H:8]1[OH:9].C[Si](Cl)(C)C.Cl[C:24]([O:26][CH:27]1[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1)=[O:25]>N1C=CC=CC=1>[CH:27]1([O:26][C:24]([NH:17][C:3]2[C:2]([F:1])=[CH:15][N:6]([C@@H:7]3[O:14][C@H:12]([CH3:13])[C@@H:10]([OH:11])[C@H:8]3[OH:9])[C:5](=[O:16])[N:4]=2)=[O:25])[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1
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참가 물질

5

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 83262Carbonochloridic acid, cyclohexyl esterHCID 100374995'-Deoxy-5-fluorocytidine

생성물 1

HCID 53377959N4-(cyclohexyloxycarbonyl)-5'-deoxy-5-fluorocytidine수율 92%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5'-Deoxy-5-fluorocytidine (2.5 g) was dissolved in dry pyridine (20 ml). To the mixture, trimethylsilyl chloride (3.4 ml) was added dropwise at 0° C., and stirred for 30 min at room temperature. To the reaction mixture, cyclohexyl chloroformate (2.0 ml) was added in one portion at 0° C. After stirring of the mixture for 1 hour at room temperature, pyridine was evaporated under reduced pressure. The residue was then partitioned between saturated aqueous NaHCO3 and ether. The organic layer was washed with brine, dried over anhydrous MgSO4 and concentrated under reduced pressure. To the residue were added citric acid (2.0 g) and methanol (50 ml). The mixture was stirred at room temperature overnight. After removal of the solvent under reduced pressure, the residue was dissolved in CH2Cl2 /MeOH (95:5) and neutralized by aqueous NaOH. The organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by silica gel chromatography using CH2Cl2 /MeOH (20:1) as an eluent, followed by recrystallization from ethyl acetate to give N4 -(cyclohexyloxycarbonyl)-5'-deoxy-5-fluorocytidine (3.47 g:92% yield):mp. 134°-136° C., FAB-MS m/z 372 (MH+).

후처리

  1. stirringAfter stirring of the mixture for 1 hour at room temperature
  2. custompyridine was evaporated under reduced pressure
  3. customThe residue was then partitioned between saturated aqueous NaHCO3 and ether
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationconcentrated under reduced pressure
  7. additionTo the residue were added citric acid (2.0 g) and methanol (50 ml)
  8. stirringThe mixture was stirred at room temperature overnight
  9. customAfter removal of the solvent under reduced pressure
  10. dissolutionthe residue was dissolved in CH2Cl2 /MeOH (95:5)
  11. dry with materialThe organic layer was dried over anhydrous Na2SO4
  12. concentrationconcentrated under reduced pressure
  13. customThe residue was purified by silica gel chromatography
  14. customfollowed by recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-5265adf358bc4930b864486d52119043
출처 데이터셋
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05472949

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