Reaction equation
[Na].[CH3:2][C:3]([CH2:6][CH3:7])=[N:4][OH:5].[CH3:8][Si:9]([CH3:13])([CH3:12])[CH2:10]Cl>CN(C)C=O>[CH3:8][Si:9]([CH2:13][O:5][N:4]=[C:3]([CH2:6][CH3:7])[CH3:2])([CH3:12])[CH3:10]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To the above obtained dispersion of metallic sodium was added 34.8 g (0.4 mole) of methylethylketoxime and the reaction mixture was heated at 60° to 80° C. for about 180 minutes followed by removal of toluene under reduced pressure to give pasty sodium salt of methylethylketoxime. Then, this sodium salt of methylethylketoxime was dispersed in a mixture of 49.2 g (0.4 mole) of trimethylchloromethylsilane and 100 ml of N,N-dimethylformamide and heated at 70° to 80° C. for 3 hours with agitation. The reaction mixture after completion of the reaction was washed with water to remove sodium chloride formed as the by-product and N,N-dimethylformamide and the residue was extracted with diethyl ether followed by evaporation of the ether to give a crude product which was further distilled under reduced pressure to give 48.4 g of a liquid product boiling at 84° C. under 50 mmHg. This product is referred to as compound S-I hereinafter.
Workup
- temperatureheated at 70° to 80° C. for 3 hours with agitation
- washThe reaction mixture after completion of the reaction was washed with water
- customto remove sodium chloride
- customformed as the by-product and N,N-dimethylformamide
- extractionthe residue was extracted with diethyl ether
- customfollowed by evaporation of the ether
- customto give a crude product which
- distillationwas further distilled under reduced pressure
Sources & evidence
- ORD record
- ord-22e7e3704c5041a3a14f885a57b508b8
- Source dataset
- uspto-grants-1981_07
- Patent number
- US04278666
Linked notes
Loading…