Hydrochloric Acid → 5-(3'-Chloro-4'-trifluoromethoxy-phenyl-carbamoyl)-1,3-dimethyl-barbituric acid

HRID 1732882노트

반응식

HRID 1732882 반응식
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=[O:7])[N:5]([CH3:11])[C:3]1=[O:4].C(N(CC)CC)C.[Cl:19][C:20]1[CH:21]=[C:22]([N:31]=[C:32]=[O:33])[CH:23]=[CH:24][C:25]=1[O:26][C:27]([F:30])([F:29])[F:28].Cl>O1CCOCC1>[Cl:19][C:20]1[CH:21]=[C:22]([NH:31][C:32]([CH:8]2[C:9](=[O:10])[N:2]([CH3:1])[C:3](=[O:4])[N:5]([CH3:11])[C:6]2=[O:7])=[O:33])[CH:23]=[CH:24][C:25]=1[O:26][C:27]([F:30])([F:29])[F:28]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 69860Dimethylbarbituric acidHCID 15765405HCID 15765405, 화합물

생성물 1

HCID 705933255-(3'-Chloro-4'-trifluoromethoxy-phenyl-carbamoyl)-1,3-dimethyl-barbituric acid수율 83.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

7.8 g (0.05 mol) of 1,3-dimethylbarbituric acid were suspended in 150 ml of dioxane and 5 g (0.05 mol) of triethylamine, and 11.85 g (0.05 mol) of 3-chloro-4-trifluoromethoxy-phenyl isocyanate were added. The mixture was stirred for 5 hours under reflux. When it had cooled, the reaction mixture was brought to a pH value of 3 with 2 N hydrochloric acid and was concentrated in vacuo by distilling off the solvent. The residue was mixed with 200 ml of water, filtered off, mixed with 100 ml of isopropanol, again filtered off and dried. 16.5 g (74% of theory) of 5-(3'-chloro-4'-trifluoromethoxy-phenyl-carbamoyl)-1,3-dimethyl-barbituric acid, of melting point 160° C., were obtained.

후처리

  1. temperatureunder reflux
  2. temperatureWhen it had cooled
  3. concentrationwas concentrated in vacuo
  4. distillationby distilling off the solvent
  5. additionThe residue was mixed with 200 ml of water
  6. filtrationfiltered off
  7. additionmixed with 100 ml of isopropanol
  8. filtrationagain filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-4a121b65ebc44226b978f09fc019cad4
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04239762

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