HRID1800754
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 a solution of the above-mentioned crude product of methyl 3-(2-cyanoethenyl)benzoate in ethanol (45 mL)/tetrahydrofuran (15 mL) was added 10% palladium-carbon (648 mg), and the mixture was stirred at room temperature under a hydrogen atmosphere (1 atm) for 2 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10→75/25), and the fractions containing the object product were concentrated under reduced pressure to give the title compound (2.03 g, 88%) as a colorless oil.
WORKUP
后处理
- filtrationThe insoluble material was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10→75/25)
- additionthe fractions containing the object product
- concentrationwere concentrated under reduced pressure