Hydrochloric Acid → 5-(2-chlorophenyl)-4-cyclopropyl-2,4-dihydro-3H-1,2,4-triazol-3-one

HRID 660850

反応式

HRID 660850 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[C:4]([NH:6][NH:7][C:8]([NH:10][CH:11]1[CH2:13][CH2:12]1)=[O:9])=O.Cl>[OH-].[Na+]>[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[C:4]1[N:10]([CH:11]2[CH2:13][CH2:12]2)[C:8](=[O:9])[NH:7][N:6]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 471621452-(2-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide

生成物 1

HCID 580121355-(2-chlorophenyl)-4-cyclopropyl-2,4-dihydro-3H-1,2,4-triazol-3-one

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

7.00 g (27.6 mmol) of 2-(2-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide from Example 10A are heated under reflux for about 60 hrs in 30 ml 3 N aqueous sodium hydroxide (conversion testing by LC/MS analysis). After cooling, it is acidified with 1 N hydrochloric acid and the mixture extracted three times with ethyl acetate. The combined organic phases are washed twice with saturated sodium hydrogen carbonate solution, dried over magnesium sulphate, filtered and concentrated. 3.32 g (48% of theory) of the target compound are thus obtained.

後処理

  1. temperatureAfter cooling
  2. extractionthe mixture extracted three times with ethyl acetate
  3. washThe combined organic phases are washed twice with saturated sodium hydrogen carbonate solution
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custom3.32 g (48% of theory) of the target compound are thus obtained

出典と根拠

ORDレコード
ord-1005fd404d3446ca93ee44b49713812a
出典データセット
uspto-grants-2011_12
特許番号
US08084481B2

関連ノート

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