反応 #487576

反応方程式

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

溶媒

THF

反応条件

後処理

1. 1
   その他the starting material was consumed (confirmed by HPLC)
2. 2
   ろ過the mixture was filtered
3. 3
   その他to remove potassium carbonate
4. 4
   濃縮The resulting filtrate was concentrated in vacuo
5. 5
   その他the solid triturated with dichlormethane and isopropyl ether
6. 6
   その他fitted
7. 7
   その他to obtain a white powder (838 mg, 67% yield, 97% purity)

実験手順

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).

出典