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Methyl iodide → 2-Amino-3-methyl-6-phenyl-4-pyrimidinone

HRID 1785440
ノート
印刷プレビュー

反応式

HRID 1785440 の反応式
[OH-].[K+].[CH3:3]I.[NH2:5][C:6]1[NH:11][C:10](=[O:12])[CH:9]=[C:8]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:7]=1>CCO>[NH2:5][C:6]1[N:11]([CH3:3])[C:10](=[O:12])[CH:9]=[C:8]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodide2 回HCID 14797Potassium HydroxideHCID 1354203652-Amino-6-phenylpyrimidin-4-ol

生成物 1

HCID 133205052-Amino-3-methyl-6-phenyl-4-pyrimidinone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of KOH (1.22 g, 22 mmol), MeI (6.85 g, 48 mmol), and 2-amino-6-phenyl-3H-pyrimidin-4-one (2.62 g, 14 mmol) in EtOH (130 mL) was stirred at room temperature in a stoppered 250 mL roundbottom flask for 3 days. An additional 6.85 g (48 mmol) MeI was added and stirring was continued for 1 day. The solvent was removed under vacuum and the residue was dissolved in H2O (35mL), warmed to 50° C., and 1N HCl was added dropwise until the solid dissolved completely. The solution was cooled to room temperature, made slightly basic with saturated NaHCO3, and the resulting white solid was filtered and dried under vacuum. M+1: 202.

後処理

  1. stirringstirring
  2. waitwas continued for 1 day
  3. customThe solvent was removed under vacuum
  4. dissolutionthe residue was dissolved in H2O (35mL)
  5. temperaturewarmed to 50° C.
  6. addition1N HCl was added dropwise until the solid
  7. dissolutiondissolved completely
  8. temperatureThe solution was cooled to room temperature
  9. filtrationthe resulting white solid was filtered
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-39cb08f716ea46fc9d7265a15ce12e7a
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07504403B2

反応ノート

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