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Ammonium formate → HCID 59375151, 화합물

HRID 662003
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HRID 662003 반응식
[CH3:1][C:2]1[C:3](=[O:35])[N:4]([C:8]2[C:9]([CH3:34])=[C:10]([C:14]3[C:26]4[C:25]5[C:20](=[CH:21][C:22]([C:27]([OH:30])([CH3:29])[CH3:28])=[CH:23][CH:24]=5)[NH:19][C:18]=4[C:17]([C:31]([NH2:33])=[O:32])=[CH:16][CH:15]=3)[CH:11]=[CH:12][CH:13]=2)[CH2:5][C:6]=1[CH3:7].C([O-])=O.[NH4+]>CO.[Pd].C(Cl)Cl>[CH3:1][CH:2]1[CH:6]([CH3:7])[CH2:5][N:4]([C:8]2[C:9]([CH3:34])=[C:10]([C:14]3[C:26]4[C:25]5[C:20](=[CH:21][C:22]([C:27]([OH:30])([CH3:29])[CH3:28])=[CH:23][CH:24]=5)[NH:19][C:18]=4[C:17]([C:31]([NH2:33])=[O:32])=[CH:16][CH:15]=3)[CH:11]=[CH:12][CH:13]=2)[C:3]1=[O:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 2723923Ammonium formate4회HCID 66606416HCID 66606416, 화합물

생성물 1

HCID 59375151HCID 59375151, 화합물수율 55%

시약·촉매·용매 3

HCID 23938Palladium촉매2회HCID 887Methanol용매HCID 6344Dichloromethane
용매

실험 절차

A mixture of 4-(3-(3,4-dimethyl-2-oxo-2,5-dihydro-1H-pyrrol-1-yl)-2-methylphenyl)-7-(2-hydroxypropan-2-yl)-9H-carbazole-1-carboxamide (Example 81-21, 20 mg, 0.043 mmol) and ammonium formate (27.0 mg, 0.428 mmol) in methanol (5 mL) was treated with 10% palladium on charcoal (20 mg, 0.019 mmol). The mixture was stirred under nitrogen at rt for 2 h. Additional ammonium formate (27.0 mg, 0.428 mmol) was added and the mixture was stirred at rt overnight. More ammonium formate (57 mg) and 10% palladium on charcoal (40 mg) were added, and after 6 h more additional ammonium formate (57 mg) was added. The mixture was again stirred overnight, then was diluted with DCM and filtered through Celite. The filtrate was washed with water, dried and concentrated. The residue was purified by preparative HPLC and the appropriate effluent fractions were made basic with 1 M aqueous sodium hydroxide and extracted twice with DCM. The combined organic phases were washed with water, dried and concentrated to provide 4-(3-(3,4-dimethyl-2-oxopyrrolidin-1-yl)-2-methylphenyl)-7-(2-hydroxypropan-2-yl)-9H-carbazole-1-carboxamide as a white solid (11 mg, 55%), which was a mixture of diastereomers. Mass spectrum m/z 452.1 (M+H—H2O)+.

후처리

  1. stirringthe mixture was stirred at rt overnight
  2. waitThe mixture was again stirred overnight
  3. filtrationfiltered through Celite
  4. washThe filtrate was washed with water
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was purified by preparative HPLC
  8. extractionextracted twice with DCM
  9. washThe combined organic phases were washed with water
  10. customdried
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c64b8144d1c946b2af4bff75304053f0
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084620B2

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