반응 #2789

반응 방정식

2-cyano-1-phosphonoethanesulfonate

hydrogen

→

3-Amino-1-phosphonopropanesulfonic Acid

용매

ammonia

반응 조건

후처리

1. 1
   workup.WAITthe mixture is hydrogenated at 40 PSI on a Parr apparatus for several hours
2. 2
   여과The catalyst is filtered off
3. 3
   기타the filtrate is evaporated
4. 4
   기타dry
5. 5
   기타The product is purified
6. 6
   workup.DISSOLUTIONby dissolving the residue in water
7. 7
   workup.ADDITIONadding ethanol
8. 8
   기타to give a precipitate
9. 9
   기타collecting the solids
10. 10
    여과by filtration
11. 11
    기타Further purification
12. 12
    기타by again recrystallizing from water/ethanol

실험 절차

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.

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