HCID 18536675, compound → HCID 18536678, compound
Reaction equation
[CH2:1]([O:3][CH:4]([O:12][CH2:13][CH3:14])[C:5](=O)[CH:6]([CH3:10])[C:7](=O)[CH3:8])[CH3:2].C(=O)(O)[O-].[C:19]1([NH:25][C:26]([NH2:28])=[NH2+:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH3:10][C:6]1[C:5]([CH:4]([O:12][CH2:13][CH3:14])[O:3][CH2:1][CH3:2])=[N:27][C:26]([NH:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:28][C:7]=1[CH3:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 75 °C
Procedure
A mixture of 44 g (purity about 50%, about 0.11 mol) of 1,1-diethoxy-3-methylpentane-2,4-dione (crude product, Example 2a) and 35 g (0.175 mol) of phenylguanidinium bicarbonate in 300 ml of ethanol was heated at 70-80° C. for about 3 hours. The reaction mixture was then concentrated and the residue was filtered, with suction, through silica gel using methyl tert-butyl ether. The solvent was evaporated. Less volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C. The residue obtained was 38 g (quantitative yield) of the title compound as a yellow oil.