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Methane → 6-[3-amino-4-[4-(2-pyrimidyl)-piperazin-1-yl]phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone

HRID 1031476
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인쇄 미리보기

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HRID 1031476 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:22]2[CH:23]([CH3:29])[CH2:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:7]=[CH:8][C:9]=1[N:10]1[CH2:15][CH2:14][N:13]([C:16]2[N:21]=[CH:20][CH:19]=[CH:18][N:17]=2)[CH2:12][CH2:11]1)([O-])=O.C>CO.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([C:22]2[CH:23]([CH3:29])[CH2:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:7]=[CH:8][C:9]=1[N:10]1[CH2:15][CH2:14][N:13]([C:16]2[N:17]=[CH:18][CH:19]=[CH:20][N:21]=2)[CH2:12][CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 297MethaneHCID 144594656-[3-nitro-4-[4-(2-pyrimidyl)-piperazin-1-yl]phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone

생성물 1

HCID 144595026-[3-amino-4-[4-(2-pyrimidyl)-piperazin-1-yl]phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone수율 30.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

2.5 g (6.3 mmol) of 6-[3-nitro-4[4-(2-pyrimidyl)-piperazin-1-yl]-phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone in 130 ml of methanol are hydrogenated under a hydrogen pressure of 5 bar in the presence of 0.3 g of palladium on active charcoal (10% Pd) at 50° C. for 3 hours. After removal of the catalyst by suction filtration, the filtrate is highly concentrated by evaporation under vacuum and the residue obtained is chromatographed on silica gel, using dichloromethane/methanol (95:5) as solvent. After concentration of the product fractions by evaporation, the residue obtained is crystallized with acetone. 0.70 g (30%) of pale beige crystals, m.p. 220° to 221° C., are obtained.

후처리

  1. customat 50° C.
  2. customfor 3 hours
  3. customAfter removal of the catalyst
  4. filtrationby suction filtration
  5. concentrationthe filtrate is highly concentrated by evaporation under vacuum
  6. customthe residue obtained
  7. customis chromatographed on silica gel
  8. customAfter concentration of the product fractions by evaporation
  9. customthe residue obtained
  10. customis crystallized with acetone

출처 및 근거

ORD 기록
ord-21d49d072f044432a5efbcc5d5ff3a8c
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954501

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