HCID 22609520、化合物 → HCID 22609554、化合物

HRID 2306793ノート

反応式

HRID 2306793 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([C:42]2[CH:47]=[C:46]([O:48][CH3:49])[C:45]([O:50][CH3:51])=[C:44]([O:52][CH3:53])[CH:43]=2)=[C:8]([CH:41]=1)[C:9]([N:11]1[CH2:17][CH2:16][CH2:15][N:14]([C:18](=[O:40])[C:19]2[CH:24]=[C:23]([N+:25]([O-])=O)[CH:22]=[CH:21][C:20]=2[C:28]2[CH:33]=[C:32]([O:34][CH3:35])[C:31]([O:36][CH3:37])=[C:30]([O:38][CH3:39])[CH:29]=2)[CH2:13][CH2:12]1)=[O:10])([O-])=O>C(O)(=O)C.C(OCC)(=O)C.[Pd]>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([C:42]2[CH:43]=[C:44]([O:52][CH3:53])[C:45]([O:50][CH3:51])=[C:46]([O:48][CH3:49])[CH:47]=2)=[C:8]([CH:41]=1)[C:9]([N:11]1[CH2:17][CH2:16][CH2:15][N:14]([C:18](=[O:40])[C:19]2[CH:24]=[C:23]([NH2:25])[CH:22]=[CH:21][C:20]=2[C:28]2[CH:29]=[C:30]([O:38][CH3:39])[C:31]([O:36][CH3:37])=[C:32]([O:34][CH3:35])[CH:33]=2)[CH2:13][CH2:12]1)=[O:10]

参加物

4

反応物 1

HCID 22609520HCID 22609520、化合物

生成物 1

HCID 22609554HCID 22609554、化合物収率 95.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 22609514Ethyl acetate acetate溶媒

実験手順

Added to a solution of 39 mg (0.050 mmol) of 1,4-bis[5-nitro-2-(3,4,5-trimethoxy-phenyl)benzoyl]hexahydro-1,4-diazepine synthesized by the process described in Example 71 in acetic acid-ethyl acetate (3:2, 2.5 ml) were 39 mg of 10% palladium on carbon, and the mixture was stirred for 2 hours at room temperature under hydrogen. The catalyst was removed from the reaction mixture by suction filtration through Celite, and the filtrate was concentrated under reduced pressure. A chloroform solution of the residue was washed with a saturated aqueous solution of sodium hydrogencarbonate and a saturated saline solution, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resultant crude oil was purified by column chromatography on silica gel to obtain 32 mg (yield: 90%) of the title compound as a pale yellow amorphous powder.

後処理

  1. customsynthesized by the process
  2. customThe catalyst was removed from the reaction mixture by suction filtration through Celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. washA chloroform solution of the residue was washed with a saturated aqueous solution of sodium hydrogencarbonate
  5. dry with materiala saturated saline solution, dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resultant crude oil was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-8e46ccad1c0f460d9b6a9a9297a11934
出典データセット
uspto-grants-2004_12
特許番号
US06828316B2

反応ノート

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