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

HRID 2693

反応式

HRID 2693 の反応式
[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]

参加物

5

反応物 2

HCID 867523042-Cyano-1-phosphonoethanesulfonateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 189360993-Amino-1-phosphonopropanesulfonic Acid

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 222Ammonia溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8f0adc11e00943cfa52c22b2a6fa6941
出典データセット
uspto-grants-1998_03
特許番号
US05731299

関連ノート

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