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

HRID 1732882ノート

反応式

HRID 1732882 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 69860Dimethylbarbituric acidHCID 15765405HCID 15765405、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4a121b65ebc44226b978f09fc019cad4
出典データセット
uspto-grants-1980_12
特許番号
US04239762

反応ノート

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