Hydrochloric Acid → HCID 59394182, compound
Reaction equation
[CH3:1][C:2]1([C:5](=O)[CH2:6][C:7]#[N:8])[CH2:4][CH2:3]1.Cl.[CH3:11][NH:12][NH2:13]>CCO.O1CCOCC1>[CH3:11][N:12]1[C:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)=[CH:6][C:7]([NH2:8])=[N:13]1Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
To a solution of 3-(1-methyl-cyclopropyl)-3-oxo-propionitrile (1.0 g, 8.1 mmol) in EtOH (10 mL) is added 4N HCl in Dioxane (10 mL). The mixture is stirred at room temperature for 16 hour. Concentrated under reduced pressure, the residue is dissolved in MeOH (40 mL) and treated with methylhydrazine (0.56 g, 12.2 mmol). The mixture is heated at 80° C. for 16 h. The solution is then concentrated in vacuo and the residue is purified by HPLC give product. MS (ESI) m/z 152.3 (M+1).
Workup
- concentrationConcentrated under reduced pressure
- dissolutionthe residue is dissolved in MeOH (40 mL)
- temperatureThe mixture is heated at 80° C. for 16 h
- concentrationThe solution is then concentrated in vacuo
- customthe residue is purified by HPLC
- customgive product
Sources & evidence
- ORD record
- ord-cfb05ddc756640878fe2ff1c45642f30
- Source dataset
- uspto-grants-2013_07
- Patent number
- US08486954B2
Reaction notes
Loading…