HCID 20203459, compound → HCID 70441207, compound

HRID 978634Notes

Reaction equation

HRID 978634 reaction equation
[NH2:1][CH2:2][CH2:3][C:4]1[C:9]([NH2:10])=[CH:8][C:7]([N+:11]([O-])=O)=[CH:6][C:5]=1[S:14]([CH2:17][CH2:18][C:19]([OH:21])=[O:20])(=[O:16])=[O:15].[H][H]>O.C(O)C.[Ni]>[NH2:11][C:7]1[CH:8]=[C:9]([NH2:10])[C:4]([CH2:3][CH2:2][NH2:1])=[C:5]([S:14]([CH2:17][CH2:18][C:19]([OH:21])=[O:20])(=[O:16])=[O:15])[CH:6]=1

Participants

6

Reactant 2

HCID 20203459HCID 20203459, compoundHCID 178418361HCID 178418361, compound2×

Product 1

HCID 70441207HCID 70441207, compound

Reagents, catalysts & solvents 3

HCID 935NickelCatalystHCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

27.0 g of 3-[2-(2-aminoethyl)-amino-5-nitrophenylsulphonyl]-propionic acid are suspended in 150 ml of water and 150 ml of ethanol. In an autoclave 1 g of nickel is added to the suspension, 60-70 bar of hydrogen are injected, and the temperature is raised to 60° C. Stirring is continued for some time until no further hydrogen is absorbed. After letting down, the resultant solution is clarified at 70° C. with 1 g of activated charcoal, the clarification residue is washed with 20 ml of hot water, and the combined filtrates are reacted as per Example 10.

Workup

  1. customis absorbed
  2. customis clarified at 70° C. with 1 g of activated charcoal
  3. washthe clarification residue is washed with 20 ml of hot water
  4. customthe combined filtrates are reacted as per Example 10

Sources & evidence

ORD record
ord-68b58439b12544639fdaf5be1af46914
Source dataset
uspto-grants-1987_05
Patent number
US04665179

Reaction notes

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