Potassium Carbonate → 4,5-Diacetyl-[1,4,5]-oxadiazepine
Reaction equation
[C:1]([NH:4][NH:5][C:6](=[O:8])[CH3:7])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH3:15][CH2:16][O:17][CH2:18][CH:19](Cl)Cl>CS(C)=O>[C:1]([N:4]1[N:5]([C:6](=[O:8])[CH3:7])[CH:19]=[CH:18][O:17][CH:16]=[CH:15]1)(=[O:3])[CH3:2]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 20 °C
Procedure
A mixture of 35 g of diacetylhydrazine (0.3 mol), 124.4 g or 165.8 g of ground potassium carbonate (0.9 or 1.2 mol, respectively), 85.8 g of 2,2-dichlorodiethyl ether (0.6 mol) and 560 ml of solvent (see Table 2) is heated to 125° C. and maintained at 125-130° C. or 80-90° C. (in the case of DMSO) for 5 hours. The mixture is then cooled to 20° C. and filtered, and the filtration residue is washed with the solvent. The yield is given by the content of title compound in the combined filtrate.
Workup
- filtrationfiltered
- washthe filtration residue is washed with the solvent
Sources & evidence
- ORD record
- ord-3eddec40a65242c0868f7faf96b798b2
- Source dataset
- uspto-grants-2009_10
- Patent number
- US07598376B2
Reaction notes
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