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 61.1 g of acetonitrile and 108.3 g of methyl 1-methylcyclopropanecarboxylate was added drop-by-drop over a one-hour period to a stirred, refluxing mixture of 35.8 g of sodium hydride and 650 ml of tetrahydrofuran. The resulting mixture was stirred and refluxed for a further 18 hours, then most of the solvent was evaporated in a rotary evaporator. The residue was dissolved in 1 liter of water, and the solution was acidified with hydrochloric acid and extracted with ether. The extract was dried (MgSO4) and concentrated. The residue, a liquid, was fractionally distilled to give (1-methylcyclopropylcarbonyl)acetonitrile (D) as a colorless oil which crystallized on standing, m.p.: 32°-33° C.
WORKUP
后处理
- additionwas added drop-by-drop over a one-hour period to a stirred
- temperaturerefluxing
- temperaturerefluxed for a further 18 hours
- custommost of the solvent was evaporated in a rotary evaporator
- dissolutionThe residue was dissolved in 1 liter of water
- extractionextracted with ether
- dry with materialThe extract was dried (MgSO4)
- concentrationconcentrated
- distillationThe residue, a liquid, was fractionally distilled