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
The hydrogenation of 2-cyano-1-phosphonoethanesulfonate is carried out using the hydrogenation technique of Freifelder (J. Am. Chem. Soc., 82, 2386 (1960)). The cyano compound (2.15 g; 0.01 mole) is placed in 20 ml of 10% methanolic ammonia. Rhodium on alumina (5%) catalyst (0.5 g) is added, and the mixture is hydrogenated at 40 PSI on a Parr apparatus for several hours (until uptake of hydrogen is complete). The catalyst is filtered off, and the filtrate is evaporated dry. The product is purified by dissolving the residue in water, adding ethanol to give a precipitate, and collecting the solids by filtration. Further purification is accomplished by again recrystallizing from water/ethanol.
WORKUP
后处理
- waitthe mixture is hydrogenated at 40 PSI on a Parr apparatus for several hours
- filtrationThe catalyst is filtered off
- customthe filtrate is evaporated
- customdry
- customThe product is purified
- dissolutionby dissolving the residue in water
- additionadding ethanol
- customto give a precipitate
- customcollecting the solids
- filtrationby filtration
- customFurther purification
- customby again recrystallizing from water/ethanol