HRID2693

反应详情

EQUATION

反应方程式

HRID 2693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. waitthe mixture is hydrogenated at 40 PSI on a Parr apparatus for several hours
  2. filtrationThe catalyst is filtered off
  3. customthe filtrate is evaporated
  4. customdry
  5. customThe product is purified
  6. dissolutionby dissolving the residue in water
  7. additionadding ethanol
  8. customto give a precipitate
  9. customcollecting the solids
  10. filtrationby filtration
  11. customFurther purification
  12. customby again recrystallizing from water/ethanol