Sulfuric Acid → HCID 13823244、化合物

HRID 2231189ノート

反応式

HRID 2231189 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:20]2[C:25](=[O:26])[NH:24][C:23](=[O:27])[CH2:22][NH:21]2)[CH:5]=[C:6]([Cl:19])[C:7]=1[O:8][C:9]1[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=1.[C:28](Cl)(=[O:31])CC.S(=O)(=O)(O)O>C(O)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:20]2[C:25](=[O:26])[NH:24][C:23](=[O:27])[CH2:22][N:21]2[CH:28]=[O:31])[CH:5]=[C:6]([Cl:19])[C:7]=1[O:8][C:9]1[CH:10]=[CH:11][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 62324Propionyl chloride2 回HCID 13823230HCID 13823230、化合物

生成物 1

HCID 13823244HCID 13823244、化合物

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
80 °C

実験手順

1 g of 2-[3,5-dichloro-4-(4-methylsulfonylphenoxy)phenyl]hexahydro-1,2,4-triazine-3,5-dione was suspended in 10 ml of formic acid. 5 ml of propionyl chloride and 1 ml of concentrated sulfuric acid were successively added dropwise, and the mixture was stirred at 80° C. for 5 hours. After it had been cooled, a further 10 ml of propionyl chloride were added to complete the reaction, and the mixture was again heated at 80° C. for 5 hours with stirring. It was then poured onto ice-water, and the precipitate was filtered off with suction and extracted by boiling with a little toluene. The residue was recrystallized from isopropanol/diisopropyl ether, melting point 212° C., decomposition.

後処理

  1. temperatureAfter it had been cooled
  2. customthe reaction
  3. temperaturethe mixture was again heated at 80° C. for 5 hours
  4. stirringwith stirring
  5. additionIt was then poured onto ice-water
  6. filtrationthe precipitate was filtered off with suction
  7. extractionextracted
  8. customThe residue was recrystallized from isopropanol/diisopropyl ether, melting point 212° C., decomposition.

出典と根拠

ORDレコード
ord-82d35d1798d04180be3859456f30e867
出典データセット
uspto-grants-1988_11
特許番号
US04782056

反応ノート

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