HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetone → 2-{[4-(2-Chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-4-methylthiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetone | HCID 6571 | — |
| Reactant | 2-{[4-(2-Chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}-thioacetamide | HCID 13457228 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-{[4-(2-Chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-4-methylthiazole | HCID 13457206 | 16.3% |
Reaction Steps
A solution of 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}-thioacetamide (0.44 g) and chloroacetone (0.30 g) in ethanol (30 ml) was heated under reflux for 7 hours and then evaporated. The residual oil was purified by chromatography on silica (t.l.c. grade, 10 g) using dichloromethane plus 0-10% v/v ethyl acetate as eluant. Appropriate fractions were combined and evaporated and the residue triturated with diisopropyl ether. The resulting solid was collected, washed with petroleum ether (b.p. 60°-80° C.) and dried to give the title compound (78 mg), m.p. 107°-110° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04616024 |
| Source dataset | uspto-grants-1986_10 |
| ORD ID | ord-83cf82465bc24ea38044ec04b56abadd |
| Source note | uspto-grants-1986_10 |