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

HRID 4690노트

반응식

HRID 4690 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[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-875c847cb5274fd89a51931bb3c68eed
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727073

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