Sodium Acetate → Methyl-[6-(2-methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amine

HRID 1853961

반응식

HRID 1853961 반응식
CN([CH:4]=[C:5]1[C:10](=O)[CH2:9][CH2:8][N:7]([C:12]2[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=2[CH3:21])[CH2:6]1)C.[CH3:22][NH:23][C:24]([NH2:26])=[NH:25].C([O-])(=O)C.[Na+]>C(O)C.O>[CH3:22][NH:23][C:24]1[N:26]=[CH:4][C:5]2[CH2:6][N:7]([C:12]3[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=3[CH3:21])[CH2:8][CH2:9][C:10]=2[N:25]=1

참가 물질

6

반응물 3

HCID 517045Sodium AcetateHCID 673288983-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-oneHCID 178485088HCID 178485088, 화합물

생성물 1

HCID 67328824Methyl-[6-(2-methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one (12.06 gm, 41.7 mmol)[as prepared in reference 1] in Ethanol (250 ml) were added N-Methyl guanidine (12.20 gm, 167 mmol) and sodium acetate (27.32 gm, 334 mmol) and solution was heated under reflux for 12 hours. After cooling to room temperature, the reaction mixture was diluted with water, extracted with ethyl acetate. The organic layer was washed with brine, dried [sodium sulfate] and concentrated under vacuum. The crude product obtained was further purified by silica gel chromatography using 5-10% Methanol/Chloroform as eluent to give pure desired product [41] i.e., Methyl-[6-(2-methyl-5-nitro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amine as yellow solid. (Yield: 2.47 gm, 19.8%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 12 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried [sodium sulfate]
  6. concentrationconcentrated under vacuum
  7. customThe crude product obtained
  8. customwas further purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-a9814c2ba5f64cd6ba6bcc24f2c8f5bf
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962637B2

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