反应 #465959

反应方程式

methyl 4-amino-6-bromo-3-chloropyridine-2-carboxylate

NaOH

→

4-amino-6-bromo-3-chloropyridine-2-carboxylic acid

收率 34.8%

溶剂

methanol

反应条件

后处理

1. 1
   其他evaporated to dryness in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in water
3. 3
   其他After separation of the phases
4. 4
   其他The aqueous layer was evaporated to dryness
5. 5
   workup.DISSOLUTIONthe residue was dissolved in 50 mL of methanol
6. 6
   过滤filtered
7. 7
   其他The filtrate was evaporated under reduced pressure
8. 8
   其他the residue was triturated with 5 percent diethyl ether in petroleum ether

实验过程

To methyl 4-amino-6-bromo-3-chloropyridine-2-carboxylate (200mg; 0.8 mmol) in 10 mL of methanol was added excess 2N NaOH (10 mL). The mixture was stirred for 1 hr at ambient temperature and then evaporated to dryness in vacuo. The residue was dissolved in water and diethyl ether. After separation of the phases, the aqueous layer was acidified with 1N HCl to a pH=2. The aqueous layer was evaporated to dryness and the residue was dissolved in 50 mL of methanol and filtered. The filtrate was evaporated under reduced pressure and the residue was triturated with 5 percent diethyl ether in petroleum ether to give 70 mg of 4-amino-6-bromo-3-chloropyridine-2-carboxylic acid, mp 182-183° C.

来源