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

HRID 1382717
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HRID 1382717 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.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]
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참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-673b93bf2ef044958d4e1e291895f078
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04808587

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