Sodium hydride → HCID 19896217, 화합물

HRID 1196779

반응식

HRID 1196779 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19896217HCID 19896217, 화합물수율 33.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c86af5ea0fd74d728bd469c85c45b158
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116404

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