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Stannous chloride dihydrate → HCID 15907986, 화합물

HRID 1385163
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HRID 1385163 반응식
O.O.[Sn](Cl)Cl.[N:6]([CH:9]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18](=[S:34])[NH:19][C:20]2[CH:25]=[CH:24][C:23]([NH:26][C:27]([C:29]3[O:30][CH:31]=[CH:32][CH:33]=3)=[O:28])=[CH:22][CH:21]=2)=[CH:13][C:12]=1[Cl:35])[CH3:10])=[N+]=[N-]>CO.C(OCC)(=O)C>[NH2:6][CH:9]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18](=[S:34])[NH:19][C:20]2[CH:21]=[CH:22][C:23]([NH:26][C:27]([C:29]3[O:30][CH:31]=[CH:32][CH:33]=3)=[O:28])=[CH:24][CH:25]=2)=[CH:13][C:12]=1[Cl:35])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 61436Stannous chloride dihydrateHCID 22612954HCID 22612954, 화합물

생성물 1

HCID 15907986HCID 15907986, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of tin(II) chloride dihydrate (0.25 g) in methanol (2.5 mL) is added furan-2-carboxylic acid (4-{3-[4-(1-azido-ethyl)-3-chloro-phenyl]-thioureido}-phenyl)-amide (0.22 g) and the solution is stirred for approximately 15 hours at room temperature. The solution is then diluted with ethyl acetate, washed successively with saturated aqueous sodium bicarbonate then saturated aqueous sodium chloride, then dried over anhydrous sodium sulfate. After removal of the solvent by evaporation under reduced pressure the residue is chromatographed over silica gel (8% methanol in dichloromethane containing 1% triethylamine is used as the eluant) to provide the desired product as a yellow solid.

후처리

  1. washwashed successively with saturated aqueous sodium bicarbonate
  2. dry with materialsaturated aqueous sodium chloride, then dried over anhydrous sodium sulfate
  3. customAfter removal of the solvent
  4. customby evaporation under reduced pressure the residue
  5. customis chromatographed over silica gel (8% methanol in dichloromethane containing 1% triethylamine

출처 및 근거

ORD 기록
ord-91c4e0a0451144fe8b31b50f79b67a4f
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06262082B1

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