Ammonium formate → FK 1052

HRID 486208노트

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HRID 486208 반응식
O[CH:2]([C:18]1[N:19]=[CH:20][N:21](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[C:22]=1[CH3:23])[CH:3]1[C:16](=[O:17])[N:7]2[C:8]3[C:13]([C:14]([CH3:15])=[C:6]2[CH2:5][CH2:4]1)=[CH:12][CH:11]=[CH:10][CH:9]=3.C([O-])=O.[NH4+]>C(O)(=O)C.[Pd]>[CH3:15][C:14]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]2[C:16](=[O:17])[CH:3]([CH2:2][C:18]3[N:19]=[CH:20][NH:21][C:22]=3[CH3:23])[CH2:4][CH2:5][C:6]=12

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 150519238,9-dihydro-7-[(hydroxy)(5-methyl-1-trityl-1H-imidazol-4-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one

생성물 1

HCID 125368FK 1052수율 76.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

To a solution of 8,9-dihydro-7-[(hydroxy)(5-methyl-1-trityl-1H-imidazol-4-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (4.6 g) in acetic acid (92 ml) were added 10% palladium on carbon (2.3 g) and ammonium formate (7.89 g), and the mixture was refluxed gently for 3 hours. After being cooled, the catalyst was filtered off. The filtrate was evaporated, and diluted with water (50 ml) and diisopropyl ether (50 ml). Aqueous sodium hydroxide was added to neutralized the solution. Resulted precipitates were collected, and washed with water and diisopropyl ether successively, to give 8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (1.87 g).

후처리

  1. temperaturethe mixture was refluxed gently for 3 hours
  2. temperatureAfter being cooled
  3. filtrationthe catalyst was filtered off
  4. customThe filtrate was evaporated
  5. additiondiluted with water (50 ml) and diisopropyl ether (50 ml)
  6. additionAqueous sodium hydroxide was added
  7. customResulted
  8. customprecipitates
  9. customwere collected
  10. washwashed with water and diisopropyl ether successively

출처 및 근거

ORD 기록
ord-de13585eda784f92b86c3f4209025953
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290785

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