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

HRID 1726583ノート

反応式

HRID 1726583 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

Intermediate 98, 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.

後処理

  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

出典と根拠

ORDレコード
ord-84f79fefc4a249c6a8608dd1c49a6e13
出典データセット
uspto-grants-2009_02
特許番号
US07491819B1

反応ノート

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