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
A solution of 4.68 g (30 mmol) of 2,4-dihydroxy-3-nitro-pyridine in 100 ml of dimethylformamide was combined batchwise at ambient temperature with 2.88 g (60 mmol) of a 50% suspension of sodium hydride in paraffin oil and stirred for 15 minutes. Then 8.91 ml (75 mmol) of benzylbromide were added and the mixture was stirred for 24 hours at 80° C. The solution was then carefully stirred into approx. 250 ml of water and extracted three times with 70 ml of ethyl acetate. The extracts were washed with saturated sodium chloride solution, dried and evaporated down in vacuo. The residue was triturated with diethyl ether, suction filtered and dried. The product thus obtained was further processed without any purification.
WORKUP
后处理
- stirringthe mixture was stirred for 24 hours at 80° C
- extractionextracted three times with 70 ml of ethyl acetate
- washThe extracts were washed with saturated sodium chloride solution
- customdried
- customevaporated down in vacuo
- customThe residue was triturated with diethyl ether, suction
- filtrationfiltered
- customdried
- customThe product thus obtained
- customwas further processed without any purification