反应详情

To a suspension of 2-chloro-6-methylnicotinic acid (5.3 g, 30.8 mmol) in dichloromethane (100 ml) at 0° C. were added DMF (1 ml) and oxalyl chloride (3.2 ml, 36.9 mmol). The mixture was allowed to warmn to room temperature and stirred for 5 h. The solvents were removed in vacuo and the residue was dissolved in dichloromethane (50 ml) and methanol (50 ml). The mixture was stirred at room temperature for 18 h and then concentrated in vacuo. The residue was dissolved in chloroform, washed with saturated sodium bicarbonate solution and brine, dried over MgSO4, and concentrated in vacuo to give a brown oil; yield 5.70 g (100%).

1. customto warmn to room temperature
2. customThe solvents were removed in vacuo
3. dissolutionthe residue was dissolved in dichloromethane (50 ml)
4. stirringThe mixture was stirred at room temperature for 18 h
5. concentrationconcentrated in vacuo
6. dissolutionThe residue was dissolved in chloroform
7. washwashed with saturated sodium bicarbonate solution and brine
8. dry with materialdried over MgSO4
9. concentrationconcentrated in vacuo
10. customto give a brown oil