HCID 22609520, 화합물 → HCID 22609554, 화합물

HRID 1250967노트

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HRID 1250967 반응식
[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]

참가 물질

4

반응물 1

HCID 22609520HCID 22609520, 화합물

생성물 1

HCID 22609554HCID 22609554, 화합물수율 95.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 22609514Ethyl acetate acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-932125c05f8d477d9f1d96892eadedeb
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06340682B1

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