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

HRID 660850

반응식

HRID 660850 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1005fd404d3446ca93ee44b49713812a
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084481B2

연결된 노트

불러오는 중…