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

HRID 487981
ノート
印刷プレビュー

反応式

HRID 487981 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-dd549791586d4bd191de735d3f72b23d
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05298520

反応ノート

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