Hydrochloric Acid → HCID 58277326、化合物

HRID 1949229ノート

反応式

HRID 1949229 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([Cl:21])[CH:15]=3)=[CH:12][C:11]([C:22]([O:24]CC)=[O:23])=[N:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[OH-].[Li+].O.Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([Cl:21])[CH:15]=3)=[CH:12][C:11]([C:22]([OH:24])=[O:23])=[N:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

参加物

6

実験手順

5.11 g (12.9 mmol) of the compound of Example 21A are provided in 142 ml of tetrahydrofuran and, at room temperature, 3.08 g (129 mmol) of lithium hydroxide and 47 ml of water are added. The mixture is stirred at room temperature overnight and a 1N aqueous hydrogen chloride solution is subsequently added until the pH is acidic, the mixture extracted with ethyl acetate, and the organic phase is washed with water, dried over sodium sulfate, filtered and concentrated. 4.51 g (90% of theory) of the title compound are obtained.

後処理

  1. extractionthe mixture extracted with ethyl acetate
  2. washthe organic phase is washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-72873e60964743dea36c6b091c10f9be
出典データセット
uspto-grants-2013_03
特許番号
US08399682B2

反応ノート

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