Ammonium Hydroxide → (+/-)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine

HRID 349391노트

반응식

HRID 349391 반응식
[CH3:1][CH:2]([CH3:19])[CH:3]([C:9]1[CH:14]=[CH:13][C:12]([NH:15]C(=O)C)=[CH:11][CH:10]=1)[N:4]1[CH:8]=[N:7][CH:6]=[N:5]1.[NH4+].[OH-]>Cl>[CH3:1][CH:2]([CH3:19])[CH:3]([C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=1)[N:4]1[CH:8]=[N:7][CH:6]=[N:5]1

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 9903273(+/-)-N-[4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]phenyl]acetamide

생성물 1

HCID 10900053(+/-)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine수율 75.4%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
60 °C

실험 절차

A mixture of (±)-N-[4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]phenyl]acetamide (0.095 mol) in HCl (3N) (250 ml) was stirred and heated at 60° C. for 5 hours. The mixture was cooled, poured into ice, basified with concentrated NH4OH and extracted with CH2Cl2. The organic layer was dried, filtered off and evaporated. The residue was crystallized from 2-propanone/(C2H5)2O and filtered off, yielding 15.5 g (75%) of (±)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine (interm. 2; mp. 117.8° C.).

후처리

  1. temperatureThe mixture was cooled
  2. additionpoured into ice
  3. extractionextracted with CH2Cl2
  4. customThe organic layer was dried
  5. filtrationfiltered off
  6. customevaporated
  7. customThe residue was crystallized from 2-propanone/(C2H5)2O
  8. filtrationfiltered off

출처 및 근거

ORD 기록
ord-0abcdf2ad47d440c9c8eae9218999b11
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179825B2

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