Water → HCID 66816082、化合物

HRID 1754917ノート

反応式

HRID 1754917 の反応式
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]

参加物

6

反応物 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

生成物 1

HCID 66816082HCID 66816082、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-c6173fa8dc6b4d54902ebe6cbecdd332
出典データセット
uspto-grants-2015_10
特許番号
US09169254B2

反応ノート

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