Water → HCID 66816082, 화합물

HRID 1754917노트

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HRID 1754917 반응식
C([O-])([O-])=O.[K+].[K+].[C:7]([N:10]([C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][S:25]([N:28]2[CH2:49][CH2:48][C:31]3([N:35]=[C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[C:38]([O:42][C:43]([F:46])([F:45])[F:44])[CH:37]=4)[NH:33][C:32]3=[O:47])[CH2:30][CH2:29]2)(=[O:27])=[O:26])=[C:19]([CH3:50])[CH:18]=1)[CH2:11][CH2:12][O:13]C(=O)C)(=[O:9])[CH3:8].O>CO.C(Cl)Cl>[OH:13][CH2:12][CH2:11][N:10]([C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][S:25]([N:28]2[CH2:49][CH2:48][C:31]3([N:35]=[C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[C:38]([O:42][C:43]([F:45])([F:46])[F:44])[CH:37]=4)[NH:33][C:32]3=[O:47])[CH2:30][CH2:29]2)(=[O:27])=[O:26])=[C:19]([CH3:50])[CH:18]=1)[C:7](=[O:9])[CH3:8]

참가 물질

6

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 66816902Acetic acid 2-[acetyl-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-amino]-ethyl ester

생성물 1

HCID 66816082HCID 66816082, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

K2CO3 (9.1 mg, 66.0 μmol) was added to a solution of acetic acid 2-[acetyl-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-amino]-ethyl ester (28.1 mg, 44.0 μmol) in MeOH (0.5 mL). The mixture was stirred at room temperature for two hours. H2O was then added and the mixture was diluted with CH2Cl2. The organic layer was washed with saturated brine, and then dried over MgSO4 and concentrated under reduced pressure. The resulting residue was purified by column chromatography (CH2Cl2/MeOH=15/1) to give N-(2-hydroxy-ethyl)-N-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-acetamide as a white amorphous (24.0 mg, 92%).

후처리

  1. washThe organic layer was washed with saturated brine
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by column chromatography (CH2Cl2/MeOH=15/1)

출처 및 근거

ORD 기록
ord-c6173fa8dc6b4d54902ebe6cbecdd332
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169254B2

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