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Hydrochloric Acid → 4-(1H-1,2,4-Triazol-1-ylmethyl)benzenamine hydrochloride

HRID 487981
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인쇄 미리보기

반응식

HRID 487981 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][N:11]2[CH:15]=[N:14][CH:13]=[N:12]2)=[CH:6][CH:5]=1)([O-])=O.[ClH:16]>C(O)C.C(OCC)(=O)C.O.[Pd]>[ClH:16].[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][N:11]2[CH:15]=[N:14][CH:13]=[N:12]2)=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 313Hydrochloric AcidHCID 64820001-(4-Nitrobenzyl)-1H-1,2,4-triazole

생성물 1

HCID 117012794-(1H-1,2,4-Triazol-1-ylmethyl)benzenamine hydrochloride수율 100%

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

실험 절차

A solution of 1-(4-nitrophenyl)methyl-1,2,4-triazole (10.0 g, 49 mmol) in ethanol (50 ml), ethyl acetate (50 ml), 5N HCl (10 ml) and water (10 ml) was hydrogenated over 10% Pd/C (1.0 g) at 40 p.s.i., in a Parr apparatus, until an uptake of 188 p.s.i., had been observed (approx 10 mins). The catalyst was removed by filtration through hyflo and the solvent removed under vacuum. The residue was azeotroped with ethanol (×2) to give the titleamine hydrochloride (10.6 g, 100%). δ (360 MHz, D2O) 5.53 (2H, s, CH2), 7.37-7.48 (4H, m, Ar-H), 8.12 (1H, s, Ar-H), 8.66 (1H, s, Ar-H).

후처리

  1. custom(approx 10 mins)
  2. customThe catalyst was removed by filtration through hyflo
  3. customthe solvent removed under vacuum
  4. customThe residue was azeotroped with ethanol (×2)

출처 및 근거

ORD 기록
ord-dd549791586d4bd191de735d3f72b23d
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05298520

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