HCID 58277355、化合物 → HCID 58277403、化合物

HRID 1949214ノート

反応式

HRID 1949214 の反応式
C([O:8][C:9]1[CH:10]=[C:11]([C:15]2[N:19]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=3)[N:18]=[C:17]([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH:16]=2)[CH:12]=[CH:13][CH:14]=1)C1C=CC=CC=1>C(O)(=O)C.[Pd]>[Cl:26][C:22]1[CH:21]=[C:20]([N:19]2[C:15]([C:11]3[CH:12]=[CH:13][CH:14]=[C:9]([OH:8])[CH:10]=3)=[CH:16][C:17]([C:27]([O:29][CH2:30][CH3:31])=[O:28])=[N:18]2)[CH:25]=[CH:24][CH:23]=1

参加物

4

反応物 1

HCID 58277355HCID 58277355、化合物

生成物 1

HCID 58277403HCID 58277403、化合物収率 84%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

19.1 g (44.1 mmol) of the compound of Example 43A are provided in 367 ml of conc. acetic acid, 23.5 g (11.0 mmol) of palladium on activated carbon (5%) are added, and the mixture is stirred under a hydrogen atmosphere at room temperature overnight. The reaction mixture is subsequently filtered, the filtrate is concentrated, the residue is taken up in dichloromethane and washed with an aqueous sodium bicarbonate solution, and the organic phase is dried over sodium sulfate and concentrated. 12.7 g of the title compound with 63% purity (53% of theory) are obtained.

後処理

  1. filtrationThe reaction mixture is subsequently filtered
  2. concentrationthe filtrate is concentrated
  3. washwashed with an aqueous sodium bicarbonate solution
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-1b507b665854474cbfbe96005653bd37
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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