Ethanol → HCID 20183309, 화합물

HRID 255731노트

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HRID 255731 반응식
[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]([NH2:25])=[O:24].C=O.[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.[CH2:35](O)C>ClCCCl>[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]([NH:25][CH2:28][N:29]1[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][CH2:30]1)=[O:24]

참가 물질

6

반응물 4

HCID 702EthanolHCID 712FormaldehydeHCID 531671-MethylpiperazineHCID 11724425HCID 11724425, 화합물

생성물 1

HCID 20183309HCID 20183309, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A mixture of 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxamide (5 g), formalin (37%, 1.35 ml), N-methylpiperazine (2.25 g), ethanol (50 ml) and 1,2-dichloroethane (25 ml) was refluxed for 6 hours. After evaporating the solvent in vacuo, the residue was chromatographed on alumina (200 ml) and eluted with chloroform. The fractions containing the object compound were combined and concentrated under reduced pressure. The residue was recrystallized from diethyl ether to give 6-methyl-N-(4-methylpiperazin-1-ylmethyl)-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxamide (1.90 g).

후처리

  1. temperaturewas refluxed for 6 hours
  2. customAfter evaporating the solvent in vacuo
  3. customthe residue was chromatographed on alumina (200 ml)
  4. washeluted with chloroform
  5. additionThe fractions containing the object compound
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-002b837b81614d6783b6c08f9450c410
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698340

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