反応 #69763

反応方程式

1-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid

2-piperazin-1-yl-ethanol

4-Methylmorpholine

hydroxybenzotriazole

N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide

HCl

→

solid

収率 43.0%

{1-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidin-4-yl}-[4-(2-hydroxy-ethyl)-piperazin-1-yl]-methanone

収率 43.0%

溶媒

Water

DMF

反応条件

後処理

1. 1
   その他the precipitate formed
2. 2
   ろ過was filtered off
3. 3
   その他dried in vacuo
4. 4
   その他The residue was purified by silica chromatography (ethyl acetate/cyclohexane)

実験手順

1-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid 14 (50 mg, 0.13 mmol), 2-piperazin-1-yl-ethanol (17.0 mg, 0.13 mmol) and 4-Methylmorpholine (70 μL, 0.64 mmol) were dissolved in DMF (3 mL). To this mixture hydroxybenzotriazole (17.0 mg, 0.13 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide×HCl (24.0 mg, 0.13 mmol) were added and the mixture was stirred for 48 h at room temperature. Water was added to the mixture and the precipitate formed was filtered off and dried in vacuo. The residue was purified by silica chromatography (ethyl acetate/cyclohexane) to yield in a colorless solid (27.8 mg, 0.05 mmol, 43%) characterized as 15.

出典