Reaktion #71344

Reaktionsgleichung

methanesulfonic acid 6-tert-butoxycarbonylamino-pyridin-3-ylmethyl ester

N-ethylpiperazine

cesium carbonate

DMF

→

title compound

Ausbeute 90.0%

[5-(4-Ethyl-piperazin-1-ylmethyl)-pyridin-2-yl]carbamic acid tert-butyl ester

Ausbeute 90.0%

Lösungsmittel

EtOAc

H2O

Et2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with EtOAc
2. 2
   WaschenThe organic phase was washed with H2O and brine
3. 3
   Trocknendried (Na2SO4)
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated
6. 6
   Sonstigeto provide a yellow solid

Vorschrift

A mixture of methanesulfonic acid 6-tert-butoxycarbonylamino-pyridin-3-ylmethyl ester (Step 26.3) (0.8 g, 2.6 mmol), N-ethylpiperazine (0.37 mL, 2.9 mmol, 1.1 equiv), cesium carbonate (1 g, 3.2 mmol, 1.2 equiv), and DMF (10 ml) was stirred for 2 h at rt, diluted with EtOAc and H2O, and extracted with EtOAc. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated to provide a yellow solid. Trituration in Et2O afforded 0.75 g of the title compound as a white solid: ES-MS: 321.2 [M+H]+.

Quelle