2-Cyano-1-phosphonoethanesulfonate → 3-Amino-1-phosphonopropanesulfonic Acid

HRID 2693

반응식

HRID 2693 반응식
[C:1]([CH2:3][CH:4]([P:9]([OH:12])([OH:11])=[O:10])[S:5]([O-:8])(=[O:7])=[O:6])#[N:2].[H][H]>N.[Rh]>[NH2:2][CH2:1][CH2:3][CH:4]([P:9]([OH:12])([OH:11])=[O:10])[S:5]([OH:8])(=[O:6])=[O:7]

참가 물질

5

반응물 2

HCID 867523042-Cyano-1-phosphonoethanesulfonateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 189360993-Amino-1-phosphonopropanesulfonic Acid

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 222Ammonia용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f0adc11e00943cfa52c22b2a6fa6941
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731299

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