HRID1761927
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 mixture of 1.90 g of methyl 3-formyl-2-hydroxybenzoate, 3.0 g of nitroethane, 0.15 ml of piperidine and 30 ml of toluene is refluxed overnight while removing water. The reaction mixture is poured into ice-water and the aqueous mixture is extracted with ethyl acetate. The extract is washed successively with 10% hydrochloric acid and an aqueous saturated sodium chloride solution, dried and evaporated to remove solvent. The residue is recrystallized from methanol to give 2.05 g of methyl 2-hydroxy-3-(2-nitro-1-propenyl)benzoate.
WORKUP
后处理
- temperatureis refluxed overnight
- customwhile removing water
- additionThe reaction mixture is poured into ice-water
- extractionthe aqueous mixture is extracted with ethyl acetate
- washThe extract is washed successively with 10% hydrochloric acid
- dry with materialan aqueous saturated sodium chloride solution, dried
- customevaporated
- customto remove solvent
- customThe residue is recrystallized from methanol