反应详情

温度

120 °C

A mixture of 5-cyano-5-(6-chloropyridin-3-yl)-2-oxocyclohexanecarboxylic acid methyl ester (10.6 mmol) and LiCl (21.1 mmol) in 15 mL wet DMSO was heated to 120° C. under microwave conditions for 2 h. The reaction mixture was diluted with water and extracted 3 times with EtOAc. The combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using Hept/EtOAc (95/5 to 20/80) gives the desired compound as yellow solid.

1. extractionextracted 3 times with EtOAc
2. washThe combined organic layers were washed with brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. customPurification with CC (KP-SIL™ from Biotage)