反应详情

A mixture of the product from step (ii) (8.7 g) and KCN (8.28 g) in DMF (20 ml) and DMSO (20 ml) was stirred at rt for 2 h then 50° C. for 2 h. Water (150 ml) was added and stirred for 30 min. The solid obtained was filtered off and added to MeOH (150 ml), heated to reflux for 5 min then hot filtered and allowed to cool to rt. The precipitate was filtered and dried under high vacuum at 45° C., to give the subtitle compound as a brown solid, 23 g.

1. wait50° C. for 2 h
2. stirringstirred for 30 min
3. customThe solid obtained
4. filtrationwas filtered off
5. additionadded to MeOH (150 ml)
6. temperatureheated
7. temperatureto reflux for 5 min
8. filtrationthen hot filtered
9. temperatureto cool to rt
10. filtrationThe precipitate was filtered
11. customdried under high vacuum at 45° C.