Sodium Methoxide → HCID 67482916、化合物

HRID 13351

反応式

HRID 13351 の反応式
C[O-].[Na+].C([O:7][C@@H:8]1[CH2:12][N:11]([C:13](=[O:15])[CH3:14])[C@@H:10]([C:16]2[C:30]([O:31][C:32]3[CH:37]=[CH:36][C:35]([S:38]([CH3:41])(=[O:40])=[O:39])=[CH:34][CH:33]=3)=[CH:29][C:19]3[N:20]=[C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)[NH:22][C:18]=3[CH:17]=2)[CH2:9]1)(=O)C>CO>[OH:7][C@@H:8]1[CH2:12][N:11]([C:13](=[O:15])[CH3:14])[C@@H:10]([C:16]2[C:30]([O:31][C:32]3[CH:33]=[CH:34][C:35]([S:38]([CH3:41])(=[O:39])=[O:40])=[CH:36][CH:37]=3)=[CH:29][C:19]3[N:20]=[C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)[NH:22][C:18]=3[CH:17]=2)[CH2:9]1

参加物

4

実験手順

0.015 ml of 25% sodium methoxide was added to a methanol (2 ml) solution of 40 mg of trans-1-(4-acetoxy-2-(6-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone obtained in Example 325, and the reaction liquid was stirred at room temperature for 10 minutes. The solvent was evaporated away under reduced pressure, and the residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]. The solvent of the resulting fraction was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound as a white solid.

後処理

  1. customthe reaction liquid
  2. customThe solvent was evaporated away under reduced pressure
  3. customthe residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]
  4. additionThe solvent of the resulting fraction was diluted with ethyl acetate
  5. washwashed with aqueous saturated sodium bicarbonate
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe solvent was evaporated away under reduced pressure

出典と根拠

ORDレコード
ord-47517cd23cb843e58edb72042e6fbf46
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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