Methane → 5-Amino-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

HRID 1382719ノート

反応式

HRID 1382719 の反応式
[N:1]([C:4]1[C:13]2[C:12](=[O:14])[N:11]([CH3:15])[C:10](=[O:16])[N:9]([CH3:17])[C:8]=2[N:7]=[CH:6][CH:5]=1)=[N+]=[N-].C>CO.[Pd]>[NH2:1][C:4]1[C:13]2[C:12](=[O:14])[N:11]([CH3:15])[C:10](=[O:16])[N:9]([CH3:17])[C:8]=2[N:7]=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 297MethaneHCID 14304685HCID 14304685、化合物

生成物 1

HCID 132683465-Amino-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione収率 74%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

1.33 g of Compound 3 was dissolved in 400 ml of methanol and reduced in the presence of 300 mg of Pd-C. Activated charcoal powder was added, and the solution was heated and filtered. The filtrate was distilled under reduced pressure and ethanol added thereto. The resulting crude crystals were separated by filtration and recrystallized from ethanol to give 0.87 g of 5-amino-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4-dione (Compound 4).

後処理

  1. temperaturethe solution was heated
  2. filtrationfiltered
  3. distillationThe filtrate was distilled under reduced pressure and ethanol
  4. additionadded
  5. customThe resulting crude crystals were separated by filtration
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-791360420a244b76ab2a826578cbd435
出典データセット
uspto-grants-1989_02
特許番号
US04808587

反応ノート

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