Hydrochloric Acid → HCID 58277435、化合物

HRID 1949255ノート

反応式

HRID 1949255 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[C:15]([Cl:20])[CH:14]=3)=[CH:11][C:10]([C:21]([O:23]CC)=[O:22])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Li+].O.Cl>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[C:15]([Cl:20])[CH:14]=3)=[CH:11][C:10]([C:21]([OH:23])=[O:22])=[N:9]2)[CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 58277324HCID 58277324、化合物

生成物 1

HCID 58277435HCID 58277435、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

688 mg of the compound of Example 51A with 76% purity (1.23 mmol) are provided in 29 ml of tetrahydrofuran and, at room temperature, 389 mg (16.2 mmol) of lithium hydroxide and 10 ml of water are added. The mixture is stirred at room temperature for 5 h, a 1N aqueous hydrogen chloride solution is subsequently added until the pH is acidic, and the mixture is extracted with ethyl acetate, dried over sodium sulfate, filtered and concentrated. The residue is stirred in a little cyclohexane and the precipitate is collected by suction filtration. 413 mg (83% of theory) of the title compound are obtained.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. stirringThe residue is stirred in a little cyclohexane
  6. filtrationthe precipitate is collected by suction filtration

出典と根拠

ORDレコード
ord-a8a8655ac1594722bace3b68c215e1ca
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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