Hydrazine hydrate (1:1) → 5-Aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

HRID 4690ノート

反応式

HRID 4690 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[CH2:23][N:24]1C(=O)C2=CC=CC=C2C1=O.O.NN>C(O)C>[NH2:24][CH2:23][C:3]1[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)=[N:5][C:6]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)=[N:7][C:2]=1[CH3:1]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 201514046-Methyl-4-(3-nitrophenyl)-5-phthalimidomethyl-2-phenylpyrimidine

生成物 1

HCID 201514135-Aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine収率 22.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 6-methyl-4-(3-nitrophenyl)-5-phthalimidomethyl-2-phenylpyrimidine (6.9 g) and hydrazine monohydrate (0.8 g) in ethanol (140 ml) was refluxed for 6 hours. After filtering off the insolubles, the filtrate was poured into a suspension of chloroform (200 ml) and water (300 ml) under stirring. The organic layer was separated, washed with aqueous sodium chloride and dried over magnesium sulfate. The solvent was evaporated in vacuo and the resulting crystals were recrystallized from ethanol to give 5-aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.12 g).

後処理

  1. temperaturewas refluxed for 6 hours
  2. filtrationAfter filtering off the insolubles
  3. additionthe filtrate was poured into a suspension of chloroform (200 ml) and water (300 ml)
  4. customThe organic layer was separated
  5. washwashed with aqueous sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was evaporated in vacuo
  8. customthe resulting crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-875c847cb5274fd89a51931bb3c68eed
出典データセット
uspto-grants-1988_02
特許番号
US04727073

反応ノート

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