反应详情

A solution of 4-(piperidin-4-ylmethyl)-phenylamine (0.57 g, 3 mmol) in dicholoromethane (20 mL) was cooled in an ice bath under nitrogen atmosphere. Isopropyl isocyanate (0.28 g, 3.3 mmol) was added dropwise to the solution and stirred at ice bath temperature for 30 minutes. The reaction mixture was quenched with water and extracted with dichloromethane. The combined organic extracts were washed with water and brine, dried, and solvents removed in vacuo. The crude product was chromatographed on silica gel, eluting with 2% methanovdichloromethane containing 0.01% ammonium hydroxide, to give 4-(1-isopropylaminocarbonylpiperidin-4-ylmethyl)-phenylamine (0.66 g, 80%) as a gum.

1. customThe reaction mixture was quenched with water
2. extractionextracted with dichloromethane
3. washThe combined organic extracts were washed with water and brine
4. customdried
5. customsolvents removed in vacuo
6. customThe crude product was chromatographed on silica gel
7. washeluting with 2% methanovdichloromethane
8. additioncontaining 0.01% ammonium hydroxide