反应详情

温度

80 °C

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

1. additionis added over 5 minutes
2. temperaturethe mixture is cooled
3. customThe solid obtained
4. filtrationis filtered off
5. washrinsed with 3×200 ml of acetonitrile
6. dissolutiondissolved in 800 ml of isopropanol (at reflux)
7. temperatureAfter cooling
8. addition1 l of ethyl ether is added
9. customThe precipitate formed
10. filtrationis filtered off
11. washrinsed with 3×200 ml of ethyl ether
12. customdried
13. customThe off-white powder obtained (73.77 g)