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Ammonium formate → HCID 19423601, 화합물

HRID 743079
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HRID 743079 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[CH:19]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:18]3[CH:26]=[N:27][CH:28]=[CH:29][C:17]=3[NH:16][C:15]2=[O:30])[CH2:10][CH2:9]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.[C].[Pd]>[NH:8]1[CH2:9][CH2:10][CH:11]([N:14]2[CH:19]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:18]3[CH:26]=[N:27][CH:28]=[CH:29][C:17]=3[NH:16][C:15]2=[O:30])[CH2:12][CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 9865626HCID 9865626, 화합물

생성물 1

HCID 19423601HCID 19423601, 화합물

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

To a solution of 4.13.g (10.4 mmol) of 3-(1-benzylpiperidin-4-yl)-4-phenyl-2-oxo-1,2,3,4-tetrahydropyrido[4,3-d]pyrimidine in 250 mL of methanol were added 1.89 g (30 mmol) of ammonium formate and 0.3 g of 10% palladium-carbon, and the mixture was heated under reflux for 5 hours. After being cooled, the reaction mixture was filtered through cerite, and the filtrate was concentrated in vacuo. To the residue was added an aqueous saturated sodium hydrogencarbonate solution, and the mixture was extracted with chloroform. The organic layer separated was dried on potassium carbonate and then concentrated in vacuo. The residue was purified by means of column chromatography (silica gel, 10:100:900 aqueous ammonia methanol:chloroform) to give 2.67 g (8.66 mmol) of the title compound.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. temperatureAfter being cooled
  4. filtrationthe reaction mixture was filtered through cerite, and the filtrate
  5. concentrationwas concentrated in vacuo
  6. additionTo the residue was added an aqueous saturated sodium hydrogencarbonate solution
  7. extractionthe mixture was extracted with chloroform
  8. customThe organic layer separated
  9. customwas dried on potassium carbonate
  10. concentrationconcentrated in vacuo
  11. customThe residue was purified by means of column chromatography (silica gel, 10:100:900 aqueous ammonia methanol:chloroform)

출처 및 근거

ORD 기록
ord-f92faf9b39d84d58ae2d8efdf1d8be8d
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05556860

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