반응 #487576

반응 방정식

2-chloroethyl isocyanate

3-(4-aminopiperidin-1-ylsulfonyl)-4-(3,5-dichlorophenoxy)benzonitrile

potassium carbonate

→

3-(4-aminopiperidin-1-ylsulfonyl)-4-(3,5-dichlorophenoxy)benzonitrile

final product

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

용매

THF

반응 조건

후처리

1. 1
   기타the starting material was consumed (confirmed by HPLC)
2. 2
   여과the mixture was filtered
3. 3
   기타to remove potassium carbonate
4. 4
   농축The resulting filtrate was concentrated in vacuo
5. 5
   기타the solid triturated with dichlormethane and isopropyl ether
6. 6
   기타fitted
7. 7
   기타to obtain a white powder (838 mg, 67% yield, 97% purity)

실험 절차

3-(4-aminopiperidin-1-ylsulfonyl)-4-(3,5-dichlorophenoxy)benzonitrile was prepared following the procedure of Example 1. The final product was prepared by dissolving 3-(4-aminopiperidin-1-ylsulfonyl)-4-(3,5-dichlorophenoxy)benzonitrile (1.00 g) in THF (30 mL) followed by the addition potassium carbonate (975 mg, 3.0 eq.), then 2-chloroethyl isocyanate (496 mg, 2.0 eq.) dropwise. After stirring for 1 hour, the starting material was consumed (confirmed by HPLC), and the mixture was filtered to remove potassium carbonate. The resulting filtrate was concentrated in vacuo, the solid triturated with dichlormethane and isopropyl ether, and fitted to obtain a white powder (838 mg, 67% yield, 97% purity).

출처