Dimethylformamide → 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione

HRID 328120

반응식

HRID 328120 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([N:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13](=[O:20])[NH:12][C:11]2=[O:21])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH3:22]N(C)C=O.[H-].[Na+].S(OC)(OC)=O>O>[N+:1]([C:4]1[CH:5]=[C:6]([N:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13](=[O:20])[N:12]([CH3:22])[C:11]2=[O:21])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 69223Dimethyl sulfiteHCID 128123771-(m-nitrophenyl)quinazoline-2,4(1H, 3H)-dione

생성물 1

HCID 128123781-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 2.8 g of 1-(m-nitrophenyl)quinazoline-2,4(1H, 3H)-dione and 30 ml of dimethylformamide was added 0.6 g of approximately 55 % sodium hydride, and the solution was stirred for 20 minutes at room temperature. To this was added 2.2 g of dimethyl sulfite and stirring was further continued for 4 hours at room temperature. After the reaction was complete, the solvent was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was mixed with water to precipitate a crude product. This product was recrystallized from methanol to afford 2.8 g of 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 242°-243° C.

후처리

  1. stirringstirring
  2. waitwas further continued for 4 hours at room temperature
  3. customthe solvent was removed from the reaction mixture by distillation under reduced pressure
  4. customThe residue thus obtained
  5. customto precipitate a crude product
  6. customThis product was recrystallized from methanol

출처 및 근거

ORD 기록
ord-0c4cbc72e24d4188a445601834301607
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04016166

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