Water → 3-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

HRID 1287245

반응식

HRID 1287245 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([N:10]2[C:15]3[N:16]=[CH:17][CH:18]=[CH:19][C:14]=3[C:13](=[O:20])[NH:12][C:11]2=[O:21])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[H-].[Na+].[CH2:24](OS(OCC)=O)[CH3:25].O>CN(C)C=O>[N+:1]([C:4]1[CH:5]=[C:6]([N:10]2[C:15]3[N:16]=[CH:17][CH:18]=[CH:19][C:14]=3[C:13](=[O:20])[N:12]([CH2:24][CH3:25])[C:11]2=[O:21])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 12197Sulfurous acid, diethyl esterHCID 24758Sodium hydrideHCID 127603011-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 127641783-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione수율 87.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.8 g of 1-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione was dissolved in 30 ml of dry dimethylformamide. To the solution was added 0.6 g of about 50 % sodium hydride, and stirring was performed for 30 minutes. To the mixture was further added 3.5 g of diethylsulfite and the whole was reacted for 2 hours at room temperature. After the reaction was finished, the solvent was distilled off from the mixture under reduced pressure. To the residue thus obtained was added water to precipitate a crude product. This product was recrystallized from methanol to yield 2.7 g of 1-(m-nitrophenyl)-3-ethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione as pale yellow prisms, melting at 210°-211°C.

후처리

  1. customthe whole was reacted for 2 hours at room temperature
  2. distillationthe solvent was distilled off from the mixture under reduced pressure
  3. customTo the residue thus obtained
  4. customto precipitate a crude product
  5. customThis product was recrystallized from methanol

출처 및 근거

ORD 기록
ord-e3bf5f87350d4fe59f8c16d9f847409a
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03984415

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