Reacción #1885113

Ecuación de reacción

2-(1,4-diaza-bicyclo[3.2.2]non-4-yl)-pyrimidin-5-ylamine

2-nitrobenzoylchloride

→

N-[2-(1,4-Diaza-bicyclo[3.2.2]non-4-yl)-pyrimidin-5-yl]-2-nitro-benzamide hydrochloric acid salt

Disolventes

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   FiltraciónThe crystals were filtered
2. 2
   Lavadowashed with THF
3. 3
   workup.WAITthe mixture was stored in the refrigerator for 3 hours
4. 4
   FiltraciónThe crystals were filtered
5. 5
   Lavadowashed with ethanol

Procedimiento

A mixture of 2-(1,4-diaza-bicyclo[3.2.2]non-4-yl)-pyrimidin-5-ylamine free base and THF (275 ml) was added to another mixture of 2-nitrobenzoylchloride (10 g, 53.9 mmol) during 45 minutes. The mixture was stirred at room temperature for 15 h. The crystals were filtered and washed with THF. The crystals where boiled in ethanol (100 ml, 96%) and the mixture was stored in the refrigerator for 3 hours. The crystals were filtered and washed with ethanol followed by diethylether. Yield 6.47 g (33%). LC-ESI-HRMS of [M+H]+ shows 369.169 Da. Calc. 369.167514 Da, dev. 4 ppm.

Fuente