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

HRID 1382717
ノート
印刷プレビュー

反応式

HRID 1382717 の反応式
Cl[C:2]1[C:11]2[C:10](=[O:12])[N:9]([CH3:13])[C:8](=[O:14])[N:7]([CH3:15])[C:6]=2[N:5]=[CH:4][CH:3]=1.C>CO.[Pd]>[CH3:15][N:7]1[C:6]2[N:5]=[CH:4][CH:3]=[CH:2][C:11]=2[C:10](=[O:12])[N:9]([CH3:13])[C:8]1=[O:14]
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 2

HCID 297MethaneHCID 143046845-Chloro-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 6055851,3-Dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione収率 84%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

0.34 g of Compound 1 was dissolved in 100 ml of methanol and reduced in the presence of Pd-C. Activated charcoal powder was added, and the solution was heated and filtered. The filtrate was distilled under reduced pressure and ethanol was added thereto. The resulting crude crystals were separated from the solution by the filtration and recrystallized from ethanol to give 0.24 g of 1,3-dimethylpyrido[2,3-d]pyrimidine-2,4-dione (Compound 2).

後処理

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

出典と根拠

ORDレコード
ord-673b93bf2ef044958d4e1e291895f078
出典データセット
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04808587

反応ノート

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