These common heterocyclic compound, 4630-82-4, name is Methyl cyclohexanecarboxylate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 4630-82-4
60%-NaH (4.65g, 0. 116MOL) was suspended in DME (70mL) and then heated to 70C under reflux. Subsequently, a solution of cyclohexane carboxylic acid methyl ester (5. 00g, 0. 0352MOL) and 2-methyl-3-oxo-butyric acid ethyl ester (90%, 6.20g, 0. 0387MOL) diluted with DME (30mL) was added thereto over 45 minutes and then heated under reflux for 18 hours. After the resulting solution was cooled down to room temperature, the solvent was distilled off under reduced pressure. Then, water (50mL) was added thereto and the resulting solution was stirred for 2 hours. After a 2N HCl solution was added thereto for acidification followed by extraction with ethyl acetate (50MLX 2), the resulting organic layer was washed with a saturated NACI solution (50ML). The organic layer was dried over MGSO4, filtered, and then concentrated under a reduced pressure. The resulting residue was purified by recrystallization from ethyl acetate/n-hexane to obtain white solid (4.80g, 66%). ‘H-NMR (CDCL) ; 6 = 8. 46 (brs, 1H), 6.02 (s, 1H), 2.35 (m, 1H), 1.96 (s, 3H), 1.90- 1. 15 (m, 10H). MS = 209 [M+H], 231 [M+Na]
Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4630-82-4.
Reference:
Patent; C & C RESEARCH LABORATORIES; WO2004/50624; (2004); A1;,
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