Hydrochloric Acid → 1-[2-(1H-1,2,4-triazol-1-yl)phenyl]methanamine hydrochloride

HRID 1664151노트

반응식

HRID 1664151 반응식
[N:1]1([C:6]2[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=2[C:8]#[N:9])[CH:5]=[N:4][CH:3]=[N:2]1.[ClH:14]>C(O)C.[Pd]>[ClH:14].[N:1]1([C:6]2[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=2[CH2:8][NH2:9])[CH:5]=[N:4][CH:3]=[N:2]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 157121632-(1H-1,2,4-triazol-1-yl)Benzonitrile

생성물 1

HCID 210697781-[2-(1H-1,2,4-triazol-1-yl)phenyl]methanamine hydrochloride수율 75%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

2-(1H-1,2,4-Triazol-1-yl)benzonitrile (4.25 g, 25 mmol) was dissolved in ethanol (50 mL) and 1N HCl (25 mL). 10% Pd—C (1 g) was added and the mixture shaken under H2 for 2 h at 50 psi. After filtration through Celite® and concentration, the residue was triturated with diethyl ether and the title compound was collected as a white solid. (3.94 g, 75% yield). 1H-NMR (300 MHz, CD3OD) δ ppm: 9.01 (1H, s), 8.32 (1H, s), 7.78-7.64 (4H, m), 4.15 (2H, s). LCMS [M+H]+ calcd for C9H11N4: 175.09; found: 175.17.

후처리

  1. filtrationAfter filtration
  2. concentrationthrough Celite® and concentration
  3. customthe residue was triturated with diethyl ether
  4. customthe title compound was collected as a white solid

출처 및 근거

ORD 기록
ord-3dd60c9645164d5fa40e0245f6a79130
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039458B2

반응 노트

불러오는 중…