반응 #991

반응 방정식

(R)-4-methyl-3-pyridin-2-yl-[1,2,3]-oxathiazolidine-2,2-dioxide

4-piperazinoindole

→

(R)-1-(4-indolyl)-4-[2-methyl-2-(2-pyridinylamino)ethyl]piperazine

수율 67.5%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타then evaporated in vacuo
2. 2
   온도cooled
3. 3
   세척washed with ethyl acetate (2×100 ml)
4. 4
   추출extracted into dichioromethane (3×100 ml)
5. 5
   건조dried (MgSO4)
6. 6
   기타then evaporated in vacuo
7. 7
   기타to give a brown glass
8. 8
   기타This was purified on a silica column
9. 9
   세척eluting with 10% propan-2-ol in dichloromethane

실험 절차

A solution of (R)-4-methyl-3-pyridin-2-yl-[1,2,3]-oxathiazolidine-2,2-dioxide (4.04 g 0.019 moles) 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 HCl (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 dichioromethane (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.

출처