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

HRID 328120

反応式

HRID 328120 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c4cbc72e24d4188a445601834301607
出典データセット
uspto-grants-1977_04
特許番号
US04016166

関連ノート

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