反应 #68768
ord-633ce97e39b945cbbbe4136863d78fed
反应条件
后处理
- 1其他The solid materials formed
- 2过滤were filtered off
- 3洗涤the filtrate was washed with 1 M HCl (1 ml)
- 4干燥The organic phase was dried over MgSO4
- 5其他evaporated in vacuum
- 6其他to give 0.4 g of CT corresponding to a yield of 87%
实验过程
DCC coupling reaction was used to couple the carboxylic group of chlorambucil with the hydroxyl group of TEMPOL with the loss of a water molecule. To a stirred solution of TEMPOL (0.172 g, 1 mmol) and chlorambucil (0.304 g, 1 mmol) in methylene chloride (5 ml) at 0° C. under argon, DCC (0.206 g, 1 mmol) (Dicyclohexyl carbodiimide) and DMAP (0.0307 g, 0.25 mmol) (Dimethyl amino pyridine) were added and the reaction mixture was stirred for 12 hrs at room temperature. The solid materials formed were filtered off, and the filtrate was washed with 1 M HCl (1 ml) followed by saturated NaHCO3 (2 ml) and brine (2 ml). The organic phase was dried over MgSO4 and evaporated in vacuum to give 0.4 g of CT corresponding to a yield of 87%. TLC (Thin Layer Chromatography) of the product showed a single spot only.