반응 #487577

반응 방정식

1-(2-chloroethyl)-3-(1-(5-cyano-2-(3,5-dichlorophenoxy)-phenylsulfonyl)piperidin-4-yl)urea

potassium carbonate

morpholine

→

product

수율 65.5%

1-(1-(5-cyano-2-(3,5-dichlorophenoxy)phenylsulfonyl)piperidin-4-yl)-3-(2-morpholinoethyl)urea

수율 65.5%

용매

acetonitrile

acetone

반응 조건

후처리

1. 1
   온도heated to reflux
2. 2
   농축The mixture was then concentrated in vacuo
3. 3
   기타the solid triturated with dichlormethane and isopropyl ether
4. 4
   기타to obtain a white powder
5. 5
   온도cooled in an ice bath
6. 6
   여과filtered
7. 7
   세척washed with water

실험 절차

1-(2-chloroethyl)-3-(1-(5-cyano-2-(3,5-dichlorophenoxy)-phenylsulfonyl)piperidin-4-yl)urea (838 mg), potassium carbonate (655 mg, 3.0 eq.) and morpholine (413 mg, 3.0 eq.) were dissolved in acetonitrile (25 mL) and heated to reflux. After three hours, the reaction was complete (confirmed by HPLC). The mixture was then concentrated in vacuo, the solid triturated with dichlormethane and isopropyl ether to obtain a white powder. The powder was suspended in hot acetone, cooled in an ice bath, filtered, and washed with water to obtain the product as a white powder (601 mg, 65% yield, 97% purity).

출처