反应详情

温度

85 °C

67 g of 4-picoline were diluted in 100 ml of acetonitrile and the mixture was brought to 80° C. A mixture of 60 g of 1-bromo-2-[(2-bromoethyl)disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) was added over 5 min. After stirring for 4 h at 85° C., the mixture was cooled. The solid obtained was filtered, rinsed with 3×200 ml of acetonitrile then dissolved in 800 ml of isopropanol (under reflux). After cooling, 1 l of ethyl ether was added. The precipitate formed was filtered, rinsed with 3×200 ml of ethyl ether, then dried. The off-white powder obtained (73.77 g) very predominantly contained (>90%) the expected product which was used as such for the following step.

1. customwas brought to 80° C
2. additionwas added over 5 min
3. temperaturethe mixture was cooled
4. customThe solid obtained
5. filtrationwas filtered
6. washrinsed with 3×200 ml of acetonitrile
7. dissolutionthen dissolved in 800 ml of isopropanol (under reflux)
8. temperatureAfter cooling
9. addition1 l of ethyl ether was added
10. customThe precipitate formed
11. filtrationwas filtered
12. washrinsed with 3×200 ml of ethyl ether
13. customdried
14. customThe off-white powder obtained (73.77 g)