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HCID 21301011, 화합물 → HCID 21301002, 화합물

HRID 49975
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HRID 49975 반응식
C([N:8]1[CH2:12][CH:11]2[C:13](=[O:25])[N:14]([C:17]3[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[CH:18]=3)[C:15](=[O:16])[CH:10]2[CH2:9]1)C1C=CC=CC=1>C(O)(=O)C.[Pt]=O>[Cl:23][C:21]1[CH:22]=[C:17]([N:14]2[C:13](=[O:25])[CH:11]3[CH:10]([CH2:9][NH:8][CH2:12]3)[C:15]2=[O:16])[CH:18]=[C:19]([Cl:24])[CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 21301011HCID 21301011, 화합물

생성물 1

HCID 21301002HCID 21301002, 화합물수율 100.5%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 176Acetic Acid용매

실험 절차

A solution of 5-benzyl-2-(3,5-dichlorophenyl)-tetrahydro-pyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione (1.13 g, 3 mmol) in acetic acid (20 mL) was hydrogenated at atmospheric pressure over platinum oxide for 4 h. The catalyst was filtered off and the filtrate was poured into an ammonium hydroxide solution. The aqueous solution was extracted twice with methylene chloride. The organic layer was dried over sodium sulfate and concentrated in vacuo to give an oil (0.86 g) which was chromatographed over silica gel (CH2Cl2/MeOH/NH4OH: 90/9/1) to yield the above compound as a white solid (0.53 g). Mp=170° C. 1H NMR (DMSO-d6): 7.73 (1H, m), 7.47 (2H, m), 3.2-3.5 (4H, m), 2.8-2.9 (2H, m).

후처리

  1. filtrationThe catalyst was filtered off
  2. additionthe filtrate was poured into an ammonium hydroxide solution
  3. extractionThe aqueous solution was extracted twice with methylene chloride
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-039c11b45a7d44e1be582eb06aed2cb7
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06710064B2

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