Sodium hydride → HCID 19896217、化合物

HRID 1196779

反応式

HRID 1196779 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[NH:8][C:7](=[O:9])[NH:6][C:5](=[O:10])[CH:4]=1.[H-].[Na+].Cl[C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:19]([N+:25]([O-:27])=[O:26])=[CH:18][C:17]=1[C:28]([F:31])([F:30])[F:29]>CN(C)C=O>[N+:25]([C:19]1[CH:20]=[C:21]([N+:22]([O-:24])=[O:23])[CH:16]=[C:17]([C:28]([F:29])([F:30])[F:31])[C:18]=1[N:8]1[C:3]([C:2]([F:1])([F:11])[F:12])=[CH:4][C:5](=[O:10])[NH:6][C:7]1=[O:9])([O-:27])=[O:26]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-HCID 2338906-(Trifluoromethyl)uracil

生成物 1

HCID 19896217HCID 19896217、化合物収率 33.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

1.0 g of 6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione was added to 10 ml of dimethylformamide, followed by addition of 0.65 g of sodium hydride (purity: 55%) with stirring at 0° C. The mixed solution was stirred at room temperature for 30 minutes, then cooled to 0° C. and added dropwise with a 5 ml dimethylformamide solution of 1.89 g of 2-chloro-3,5-dinitrobenzotrifluoride. After the solution was further stirred at room temperature for 3 hours, the solvent was distilled away under reduced pressure. After addition of cooled dilute hydrochloric acid thereto, the residue was extracted with 100 ml of ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate and then the solvent was distilled away under reduced pressure to form a crude product. This crude product was recrystallized from a mixed solvent of chloroform and petroleum ether to obtain 0.77 g of the objective compound.

後処理

  1. stirringThe mixed solution was stirred at room temperature for 30 minutes
  2. temperaturecooled to 0° C.
  3. stirringAfter the solution was further stirred at room temperature for 3 hours
  4. distillationthe solvent was distilled away under reduced pressure
  5. additionAfter addition
  6. temperatureof cooled dilute hydrochloric acid
  7. extractionthe residue was extracted with 100 ml of ethyl acetate
  8. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
  9. distillationthe solvent was distilled away under reduced pressure
  10. customto form a crude product
  11. customThis crude product was recrystallized from a mixed solvent of chloroform and petroleum ether

出典と根拠

ORDレコード
ord-c86af5ea0fd74d728bd469c85c45b158
出典データセット
uspto-grants-1992_05
特許番号
US05116404

関連ノート

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