反応 #7009

反応方程式

Diisopropylethylamine

1-pyrimidin-2-yl-piperidine-4-carboxylic acid

1-hydroxybenzotriazole hydrate

3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride

→

title compound

収率 46.4%

1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N′-(3-methyl-butyryl)-hydrazide

収率 46.4%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The solvent was evaporated
2. 2
   その他the residue was triturated with water

実験手順

The residue was added to a mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (6.6 g, 31.7 mmol) (see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (4.28 g, 31.7 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (6.09 g, 31.7 mmol) in dichloromethane (50 ml). Diisopropylethylamine (17 ml, 95 mmol) was added and the mixture was stirred for 3 days. The solvent was evaporated and the residue was triturated with water and then with diethyl ether to give the title compound as a white solid (4.49 g).

出典