ethyl 1-methyl-3-oxo-cyclohexane-1-carboxylate synthesis
- Product Name:ethyl 1-methyl-3-oxo-cyclohexane-1-carboxylate
- CAS Number:7356-04-9
- Molecular formula:C10H16O3
- Molecular Weight:0
64-17-5
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Yield:-
Reaction Conditions:
at 68; for 72 h;
Steps:
43
Preparation 43 i -Methyl-3-oxo-cyclohexanecarboxylic acid ethyl ester Acetyl chloride (15.4 ml) was added dropwise to 30 ml EtOH with cooling. The product of Preparation 42 was added as a solution in EtOH (15 ml) and the reaction mixture was heated to 680C for 72 hours. The reaction mixture was cooled to ambient temperature and the solids were removed by filtration. The filtrate was concentrated in vacuo, co-evaporated twice with toluene (30 ml) and DCM (20 ml) to give 3.92 g of a brown oil. The product was purified by flash chromatography of silica gel eluting with 2:1 Hept-EtOAc. 1.72 g of product was obtained as a yellow oil. GCMS: [M+] 184.
References:
WO2009/153720,2009,A1 Location in patent:Page/Page column 224
1193-18-6
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