HRID378777
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
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.
WORKUP
后处理
- customevaporated to dryness in vacuo
- dissolutionThe residue was dissolved in water
- customAfter separation of the phases
- customThe aqueous layer was evaporated to dryness
- dissolutionthe residue was dissolved in 50 mL of methanol
- filtrationfiltered
- customThe filtrate was evaporated under reduced pressure
- customthe residue was triturated with 5 percent diethyl ether in petroleum ether