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

HRID 1382720노트

반응식

HRID 1382720 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-2c22c547a15740af85438460200dcb28
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04808587

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