HCID 70442022, compound → HCID 70440952, compound

HRID 978637Notes

Reaction equation

HRID 978637 reaction equation
[CH2:1]([S:8]([C:11]1[CH:16]=[C:15]([N+:17]([O-])=O)[CH:14]=[C:13]([NH2:20])[C:12]=1[CH2:21][CH2:22][NH2:23])(=[O:10])=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H][H]>C(O)C.O.[Ni]>[CH2:1]([S:8]([C:11]1[CH:16]=[C:15]([NH2:17])[CH:14]=[C:13]([NH2:20])[C:12]=1[CH2:21][CH2:22][NH2:23])(=[O:10])=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

6

Reactant 2

HCID 70442022HCID 70442022, compoundHCID 178418361HCID 178418361, compound2×

Product 1

HCID 70440952HCID 70440952, compound

Reagents, catalysts & solvents 3

HCID 935NickelCatalystHCID 702EthanolSolventHCID 962WaterSolvent

Procedure

20.0 g of 2-(2-aminoethyl)-amino-5-nitrophenyl benzyl sulphone are suspended in 100 ml of ethanol and 100 ml of water. In an autoclave 1 g of Raney nickel is added, 40 bar of hydrogen are injected, and the temperature is raised to 60° C. until after a further injection of hydrogen there is no further consumption. After the reduction has ended the resultant solution is clarified hot from Raney nickel, the nickel residue is washed with 40 ml of hot water, and the resulting solution is reacted as per Example 16.

Workup

  1. customno further consumption
  2. washthe nickel residue is washed with 40 ml of hot water
  3. customthe resulting solution is reacted as per Example 16

Sources & evidence

ORD record
ord-2022c533eb9c4136a13b2b8ef8555a35
Source dataset
uspto-grants-1987_05
Patent number
US04665179

Reaction notes

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