反応 #1492240

反応方程式

4-chloro-6-methyl-5-(6-amino-pyridin-3-ylethynyl)-pyrimidin-2-ylamine

piperidin-3-yl-carbamic acid tert-butyl ester

ethyl acetate

Na2CO3

→

title compound

{1-[2-Amino-5-(6-amino-pyridin-3-ylethynyl)-6-methyl-pyrimidin-4-yl]-piperidin-3-yl}-carbamic acid tert-butyl ester

溶媒

NMP

DMSO

反応条件

後処理

1. 1
   その他the phases are separated
2. 2
   抽出The aqueous phase is extracted 2 times with ethyl acetate (100 mL each)
3. 3
   乾燥The combined organic layers are dried over sodium sulfate
4. 4
   その他the solvent is removed under reduced pressure
5. 5
   その他The crude product is used without further purification in the next step

実験手順

The title compound is synthesized according to general procedure GP7 starting from 2.0 g (7.7 mmol) 4-chloro-6-methyl-5-(6-amino-pyridin-3-ylethynyl)-pyrimidin-2-ylamine and 2.0 g (10.0 mmol) piperidin-3-yl-carbamic acid tert-butyl ester using 1.29 mL (9.2 mmol) triethylamine in 5 mL NMP and 5 mL DMSO. 200 mL ethyl acetate and 100 mL half concentrated aqueous Na2CO3 solution are added and the phases are separated. The aqueous phase is extracted 2 times with ethyl acetate (100 mL each). The combined organic layers are dried over sodium sulfate and the solvent is removed under reduced pressure. The crude product is used without further purification in the next step.

出典