6-Amino-3-butyl-5-nitro-phthalide → 5,6-Diamino-3-butyl-phthalide
Reaction equation
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([CH2:12][CH2:13][CH2:14][CH3:15])[O:7][C:8]2=[O:9])=[CH:4][C:3]=1[N+:16]([O-])=O.[H][H]>C(O)C.[Ni]>[NH2:16][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[NH2:1])[C:8](=[O:9])[O:7][CH:6]2[CH2:12][CH2:13][CH2:14][CH3:15]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
To a suspension of 3.75 g (15 mmol) of compound obtained in Example 22 in 150 ml of 95% ethanol there is added Raney nickel catalyst to hydrogenate at a hydrogen pressure of 1 kg/cm2. After the absorption of hydrogen has ceased, the catalyst is filtered off, and the filtrate is concentrated to dryness. The residue is crystallised from dilute ethanol, giving the title product.
Workup
- customAfter the absorption of hydrogen
- filtrationthe catalyst is filtered off
- concentrationthe filtrate is concentrated to dryness
- customThe residue is crystallised from dilute ethanol
Sources & evidence
- ORD record
- ord-4e5c8472d63e408cadda75bf8fb62825
- Source dataset
- uspto-grants-2004_02
- Patent number
- US06689808B2
Reaction notes
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