反应详情

温度

60 °C

A solution of (R)-4-methyl-3-pyridin-2-yl-[1,2,3]-oxathiazolidine-2,2-dioxide (4.04 g 0.019 moles) prepared according to Example 1 and 4-piperazinoindole (3.80 g 0.019 moles) in acetonitrile (200 ml) was heated to 60° C. for 0.5 h then evaporated in vacuo. The residue was taken up into dilute hydrochloric acid (100 ml), warmed to 60° C. for 0.5 h, cooled, washed with ethyl acetate (2×100 ml), made basic with potassium carbonate, extracted into dichloromethane (3×100 ml), dried (MgSO4) then evaporated in vacuo to give a brown glass. This was purified on a silica column eluting with 10% propan-2-ol in dichloromethane to give (R)-1-(4-indolyl)-4-[2-methyl-2-(2-pyridinylamino)ethyl]piperazine (4.3 g) as a clear glass.

1. customthen evaporated in vacuo
2. temperaturewarmed to 60° C. for 0.5 h
3. temperaturecooled
4. washwashed with ethyl acetate (2×100 ml)
5. extractionextracted into dichloromethane (3×100 ml)
6. dry with materialdried (MgSO4)
7. customthen evaporated in vacuo
8. customto give a brown glass
9. customThis was purified on a silica column
10. washeluting with 10% propan-2-ol in dichloromethane