Methylamine → Pyrido(2,3-d)pyrimidine-2,4(1H,3H)-dione, 1,3-dimethyl-5-(methylamino)-

HRID 1382720ノート

反応式

HRID 1382720 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.[CH3:16][NH2:17]>CN(C=O)C>[CH3:16][NH:17][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

参加物

4

反応物 2

HCID 6329MethylamineHCID 143046845-Chloro-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 3086957Pyrido(2,3-d)pyrimidine-2,4(1H,3H)-dione, 1,3-dimethyl-5-(methylamino)-収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.4 g of Compound 1 and 1.86 g of methylamine (30% methanol solution) were added to 10 ml of DMF. The solution was stirred 2 hr at room temperature and the solvent was distilled off under reduced pressure. After adding water, the resulting crude crystals were separated by filtration and recrystallized from ethyl acetate to give 0.23 g of 5-methylamino-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4-dione (Compound 7)

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionAfter adding water
  3. customthe resulting crude crystals were separated by filtration
  4. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-2c22c547a15740af85438460200dcb28
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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