Stannous chloride dihydrate → HCID 178503701, 화합물

HRID 2094273노트

반응식

HRID 2094273 반응식
[Cl:1][C:2]1[CH:34]=[CH:33][C:5]2[NH:6][C:7]([C@@H:9]([NH:14][C:15](=[O:32])[C:16]3[CH:21]=[CH:20][C:19]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][C:23]4=[O:28])=[C:18]([N+:29]([O-])=O)[CH:17]=3)[CH2:10][CH2:11][S:12][CH3:13])=[N:8][C:4]=2[CH:3]=1.O.O.[Sn](Cl)Cl.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[NH2:29][C:18]1[CH:17]=[C:16]([CH:21]=[CH:20][C:19]=1[N:22]1[CH2:27][CH2:26][O:25][CH2:24][C:23]1=[O:28])[C:15]([NH:14][C@H:9]([C:7]1[NH:6][C:5]2[CH:33]=[CH:34][C:2]([Cl:1])=[CH:3][C:4]=2[N:8]=1)[CH2:10][CH2:11][S:12][CH3:13])=[O:32]

참가 물질

5

반응물 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 178503702HCID 178503702, 화합물

생성물 1

HCID 178503701HCID 178503701, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

65 mg (0.13 mmol) N-[(1S)-1-(5-chloro-1H-benzimidazol-2-yl)-3-methylsulphanyl-propyl]-4-(morpholin-3-on-4-yl)-3-nitro-benzamide dissolved in 2 ml of ethyl acetate are combined with 143 mg (0.63 mmol) tin(II)chloride-dihydrate and 130 mg (1.55 mmol) sodium hydrogen carbonate and refluxed for 2 hours. The reaction solution is combined with ice water, stirred for 10 minutes and then the precipitate formed is filtered off. After drying for 3 days the residue is purified by chromatography on silica gel (eluting gradient: dichloromethane/ethanol 100:0->91:9).

후처리

  1. temperaturerefluxed for 2 hours
  2. customthe precipitate formed
  3. filtrationis filtered off
  4. customAfter drying for 3 days the residue
  5. customis purified by chromatography on silica gel (eluting gradient: dichloromethane/ethanol 100:0->91:9)

출처 및 근거

ORD 기록
ord-3a01bb2cb90340ef84701fab726b18a8
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445525B2

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