1-ethyl-3-methyl-1H-pyrazol-4-amine → (1-Ethyl-3-methyl-1H-pyrazol-4-yl)-[2-(6-trifluoromethyl-pyridin-3-yl)-ethyl]-amine

HRID 1094392ノート

反応式

HRID 1094392 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([NH2:8])[C:5]([CH3:9])=[N:4]1)[CH3:2].[F:10][C:11]([F:22])([F:21])[C:12]1[N:17]=[CH:16][C:15]([CH2:18][C:19]#N)=[CH:14][CH:13]=1>CO.[Pd]>[CH2:1]([N:3]1[CH:7]=[C:6]([NH:8][CH2:19][CH2:18][C:15]2[CH:16]=[N:17][C:12]([C:11]([F:22])([F:10])[F:21])=[CH:13][CH:14]=2)[C:5]([CH3:9])=[N:4]1)[CH3:2]

参加物

5

反応物 2

HCID 64853541-ethyl-3-methyl-1H-pyrazol-4-amineHCID 508511273-Pyridineacetonitrile, 6-(trifluoromethyl)-

生成物 1

HCID 58007521(1-Ethyl-3-methyl-1H-pyrazol-4-yl)-[2-(6-trifluoromethyl-pyridin-3-yl)-ethyl]-amine収率 13%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 1-ethyl-3-methyl-1H-pyrazol-4-ylamine (1.345 g, 10.75 mmol, commercially available) and (6-trifluoromethyl-pyridin-3-yl)-acetonitrile (distilled 166-175° C./2 mb, 1.0 g, 5.4 mmol) in MeOH (10 mL) was treated with HCO2NH4 (1.694 g, 26.86 mmol) and 10% Pd/C (200 mg) and stirred at 80° for 1.5 h. Filtration, concentration and purification by HPLC afforded the title compound (0.213 g, 13%) as a light brown oil. MS m/e: 299.3 [M+H]+.

後処理

  1. filtrationFiltration, concentration and purification by HPLC

出典と根拠

ORDレコード
ord-5c4b8b4faffd4ba9b1da5ef83f166845
出典データセット
uspto-grants-2012_03
特許番号
US08133909B2

反応ノート

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