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

HRID 660847
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반응식

HRID 660847 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([NH:8][NH:9][C:10]([NH:12][CH:13]2[CH2:15][CH2:14]2)=[O:11])=O)=[CH:4][CH:3]=1.Cl>[OH-].[Na+]>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]2[N:12]([CH:13]3[CH2:15][CH2:14]3)[C:10](=[O:11])[NH:9][N:8]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 471338702-(4-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide

생성물 1

HCID 580121993-(4-Chlorophenyl)-4-cyclopropyl-1H-1,2,4-triazol-5(4H)-one

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

14.65 g (57.7 mmol) of 2-(4-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide from Example 2A are heated under reflux overnight in 60 ml 2 N aqueous sodium hydroxide. After cooling, the mixture is acidified to pH 1 with 2 N hydrochloric acid and extracted with ethyl acetate. The organic phase is dried over sodium sulphate, filtered and concentrated. The residue is stirred with dichloromethane, and the resulting precipitate filtered off, then washed with dichloromethane and dried in vacuo. 10.9 g (69% of theory) of the target compound are thus obtained.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. filtrationthe resulting precipitate filtered off
  7. washwashed with dichloromethane
  8. customdried in vacuo
  9. custom10.9 g (69% of theory) of the target compound are thus obtained

출처 및 근거

ORD 기록
ord-0b52c528eda44a09a45af8825fd2d1bc
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084481B2

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