反应详情

1.7 g of nitro derivative (1) prepared above and about 80 ml of methanol were introduced into a 200 ml autoclave (hydrogenator) equipped with a magnetic stirrer. The solution obtained was degassed with nitrogen. 0.2 g of palladium-on-charcoal (5% humidity, comprising 50% water) was added thereto. The reaction mixture was stirred, while flushing once with hydrogen, and hydrogen was then introduced therein at a pressure of about 5 bar. After reaction for 4 hours, the reactor was purged with nitrogen. The reaction mixture was filtered quickly through Celite under a gentle pressure of nitrogen. The filtrate: was recovered in a pre-cooled solution of methanol comprising about 3 equivalents of hydrogen chloride gas. The resulting mixture was rinsed several times with methanol under a stream of nitrogen. The concentrated solution thus obtained was then treated with ether. The product obtained, in the form of a pale pink paste, was stirred and then rinsed several times with acetonitrile and ether under nitrogen. 1.65 g of expected product (2) were isolated in the form of a slightly pink white powder. The proton and 13C NMR spectra and the microanalyses were in accordance with the expected structure of the product.

1. additionwere introduced into a 200 ml autoclave (hydrogenator)
2. customequipped with a magnetic stirrer
3. customThe solution obtained
4. customwas degassed with nitrogen
5. addition0.2 g of palladium-on-charcoal (5% humidity, comprising 50% water) was added
6. customwhile flushing once with hydrogen, and hydrogen
7. additionwas then introduced
8. customAfter reaction for 4 hours
9. customthe reactor was purged with nitrogen
10. filtrationThe reaction mixture was filtered quickly through Celite under a gentle pressure of nitrogen
11. washThe resulting mixture was rinsed several times with methanol under a stream of nitrogen
12. customThe concentrated solution thus obtained
13. customThe product obtained, in the form of a pale pink paste
14. stirringwas stirred
15. washrinsed several times with acetonitrile and ether under nitrogen