Ethanol → HCID 20183309、化合物

HRID 255731ノート

反応式

HRID 255731 の反応式
[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]

参加物

6

反応物 4

HCID 702EthanolHCID 712FormaldehydeHCID 531671-MethylpiperazineHCID 11724425HCID 11724425、化合物

生成物 1

HCID 20183309HCID 20183309、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-002b837b81614d6783b6c08f9450c410
出典データセット
uspto-grants-1987_10
特許番号
US04698340

反応ノート

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