反応 #1885113

反応方程式

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

溶媒

THF

反応条件

後処理

1. 1
   ろ過The crystals were filtered
2. 2
   洗浄washed with THF
3. 3
   workup.WAITthe mixture was stored in the refrigerator for 3 hours
4. 4
   ろ過The crystals were filtered
5. 5
   洗浄washed with ethanol

実験手順

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.

出典