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Dichloromethane methanol → HCID 90067176, 화합물

HRID 929151
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HRID 929151 반응식
I([O-])(=O)(=O)=O.[Na+].[CH2:7]([O:10][C@@H:11]1[CH2:15][O:14][C@@H:13]2[C@H:16]([O:19][C:20]3[N:21]([CH2:42][O:43][CH2:44][CH2:45][Si:46]([CH3:49])([CH3:48])[CH3:47])[C:22]4[C:23]([N:41]=3)=[N:24][C:25]([C:29]3[CH:34]=[CH:33][C:32]([C:35]5[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=5)=[CH:31][CH:30]=3)=[C:26]([Cl:28])[CH:27]=4)[CH2:17][O:18][C@H:12]12)[CH:8]=C.C[OH:51].C(Cl)Cl>C(#N)C.O.CCOC(C)=O.O.[Ru](Cl)(Cl)Cl>[Cl:28][C:26]1[CH:27]=[C:22]2[N:21]([CH2:42][O:43][CH2:44][CH2:45][Si:46]([CH3:48])([CH3:47])[CH3:49])[C:20]([O:19][C@H:16]3[C@H:13]4[O:14][CH2:15][C@@H:11]([O:10][CH2:7][CH:8]=[O:51])[C@H:12]4[O:18][CH2:17]3)=[N:41][C:23]2=[N:24][C:25]=1[C:29]1[CH:30]=[CH:31][C:32]([C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)=[CH:33][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 21226129Dichloromethane methanolHCID 23667635Sodium periodate2회HCID 90067174HCID 90067174, 화합물

생성물 1

HCID 90067176HCID 90067176, 화합물

시약·촉매·용매 4

HCID 6093376Ruthenium trichloride hydrate촉매HCID 962
Water
용매
HCID 6342Acetonitrile용매
HCID 8857Ethyl Acetate용매

실험 절차

Sodium periodate (53.4 mg, 0.250 mmol) was added to a stirred suspension of 2-[[2-[[(3R,3aR,6R,6aR)-3-allyloxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-6-yl]oxy]-6-chloro-5-(4-phenylphenyl)imidazo[4,5-b]pyridin-1-yl]methoxy]ethyl-trimethyl-silane (68.9 mg, 0.111 mmol) and ruthenium(III) chloride hydrate (1.9 mg, 8.43 μmol) in acetonitrile (0.95 ml) and water (0.16 ml). The reaction mixture was stirred at room temperature for 4 h. Additional sodium periodate (31.8 mg, 0.149 mmol) was added and the reaction mixture was stirred for 2 h at room temperature, then in the refrigerator overnight. The reaction mixture was allowed to warm to room temperature before being partitioned between EtOAc (40 ml) and saturated aqueous sodium thiosulfate (30 ml). An inseparable emulsion formed, which was filtered through a pad of Celite™. The biphasic filtrate was re-partitioned and the aqueous layer was extracted with EtOAc (2×20 ml). The organic layers were combined, washed with brine (1×15 ml), dried over MgSO4, filtered, and evaporated under reduced pressure to give a colorless residue. The residue was dissolved in EtOAc and loaded onto two 500 micron 20 cm×20 cm silica gel plates, which were developed using 10% MeOH/DCM. The silica containing the desired product band was collected and eluted with 10% MeOH/DCM (80 ml). The solvent was evaporated under reduced pressure and the resulting residue was lyophilized from ethanol and benzene to give the title compound as a white solid. LC-MS: calculated for C32H36ClN3O6Si 621.21 observed m/e: 622.31 (M+H)+ (Rt 1.34/2 min)

후처리

  1. stirringthe reaction mixture was stirred for 2 h at room temperature
  2. customin the refrigerator overnight
  3. temperatureto warm to room temperature
  4. custombefore being partitioned between EtOAc (40 ml) and saturated aqueous sodium thiosulfate (30 ml)
  5. customAn inseparable emulsion formed
  6. filtrationwhich was filtered through a pad of Celite™
  7. customThe biphasic filtrate was re-partitioned
  8. extractionthe aqueous layer was extracted with EtOAc (2×20 ml)
  9. washwashed with brine (1×15 ml)
  10. dry with materialdried over MgSO4
  11. filtrationfiltered
  12. customevaporated under reduced pressure
  13. customto give a colorless residue
  14. customThe silica containing the desired product band was collected
  15. washeluted with 10% MeOH/DCM (80 ml)
  16. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-bd01e9ec96ac48bd880e2bd378a31b7e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290517B2

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