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Water → HCID 131735095、化合物

HRID 929205
ノート
印刷プレビュー

反応式

HRID 929205 の反応式
I([O-])(=O)(=O)=O.[Na+].[Cl:7][C:8]1[CH:9]=[C:10]2[N:28]([CH2:29][O:30][CH2:31][CH2:32][Si:33]([CH3:36])([CH3:35])[CH3:34])[C:27]([O:37][C@H:38]3[C@H:42]4[O:43][CH2:44][C@@H:45]([O:46][CH2:47][CH:48]=[O:49])[C@H:41]4[O:40][CH2:39]3)=[N:26][C:11]2=[N:12][C:13]=1[C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:16][CH:15]=1.[OH2:50]>C(Cl)(Cl)(Cl)Cl.C(#N)C.CCOC(C)=O.C(Cl)Cl.CO.CC(O)=O.O.[Ru](Cl)(Cl)Cl>[Cl:7][C:8]1[CH:9]=[C:10]2[N:28]([CH2:29][O:30][CH2:31][CH2:32][Si:33]([CH3:36])([CH3:35])[CH3:34])[C:27]([O:37][C@H:38]3[C@H:42]4[O:43][CH2:44][C@@H:45]([O:46][CH2:47][C:48]([OH:50])=[O:49])[C@H:41]4[O:40][CH2:39]3)=[N:26][C:11]2=[N:12][C:13]=1[C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 3

HCID 962WaterHCID 23667635Sodium periodateHCID 90067176HCID 90067176、化合物

生成物 1

HCID 131735095HCID 131735095、化合物

試薬・触媒・溶媒 5

HCID 6093376Ruthenium trichloride hydrate触媒HCID 5943Carbon Tetrachloride溶媒
HCID 6342Acetonitrile溶媒
HCID 8857Ethyl Acetate溶媒
HCID 21877243DCM MeOH AcOH溶媒

実験手順

Sodium periodate (19.4 mg, 0.091 mmol) and ruthenium (III) chloride hydrate (1.3 mg, 5.77 μmol) were added to a stirred biphasic mixture of 2-[[(3R,3aR,6R,6aR)-6-[6-chloro-5-(4-phenylphenyl)-1-(2-trimethylsilylethoxymethyl)imidazo[4,5-b]pyridin-2-yl]oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-3-yl]oxy]acetaldehyde (13.8 mg, 0.022 mmol) in carbon tetrachloride (0.12 ml), acetonitrile (0.09 ml), and water (0.15 ml). The reaction mixture was stirred at room temperature. After 3 hours, the reaction mixture was partitioned between EtOAc (30 ml) and water (30 ml). The aqueous layer was extracted with EtOAc (2×20 ml). The organic layers were combined, washed with brine (1×20 ml), dried over MgSO4, filtered, and evaporated under reduced pressure to give a colorless residue. The residue was dissolved in EtOAc and loaded onto a 500 micron 20 cm×20 cm silica gel plate, which was developed twice using a 94:5:1 DCM/MeOH/AcOH solvent mixture (fresh solvent was used for each development). The silica containing the product band was collected and eluted with a 90:9:1 DCM/MeOH/AcOH solvent mixture (80 ml). The solvent was evaporated under reduced pressure to give the desired product as a colorless residue. LC-MS: calculated for C32H36ClN3O7Si 637.2 observed m/e: 638.33 (M+H)+ (Rt 1.35/2 min)

後処理

  1. customthe reaction mixture was partitioned between EtOAc (30 ml) and water (30 ml)
  2. extractionThe aqueous layer was extracted with EtOAc (2×20 ml)
  3. washwashed with brine (1×20 ml)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customto give a colorless residue
  8. customThe silica containing the product band was collected
  9. washeluted with a 90:9:1 DCM/MeOH/AcOH solvent mixture (80 ml)
  10. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-373c718d9ca2458abd4e274c380be580
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290517B2

反応ノート

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