反応 #487577

反応方程式

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

potassium carbonate

morpholine

→

product

収率 65.5%

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

収率 65.5%

溶媒

acetonitrile

acetone

反応条件

後処理

1. 1
   温度heated to reflux
2. 2
   濃縮The mixture was then concentrated in vacuo
3. 3
   その他the solid triturated with dichlormethane and isopropyl ether
4. 4
   その他to obtain a white powder
5. 5
   温度cooled in an ice bath
6. 6
   ろ過filtered
7. 7
   洗浄washed with water

実験手順

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).

出典