HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 10976898, compound → HCID 20277264, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 10976898 | HCID 10976898 | — |
| Reactant | 2-Chloroethyl 2-(2-cyanobenzylidene)acetoacetate | HCID 54370161 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 20277264 | HCID 20277264 | 82.5% |
Reaction Steps
A mixture of 2-chloroethyl 2-(2-cyanobenzylidene)acetoacetate (4.72 g) and ethyl 3-amino-4,4-diethoxycrotonate (4.06 g) was heated for 3 hours at 100~105° C. with stirring. After cooling, the reaction mixture was dissolved in ethyl acetate, and the solution was washed twice with an aqueous solution of sodium chloride and then dried over magnesium sulfate. After removal of the solvent under reduced pressure, the residual oil was chromatographed over silica gel with a mixture of benzene and ethyl acetate (5:1 V/V) to give 2-chloroethyl ester of 4-(2-cyanophenyl)-5-ethoxycarbonyl-6-diethoxymethyl-2-methyl-1,4-dihydropyridine-3-carboxylic acid (5.81 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04284634 |
| Source dataset | uspto-grants-1981_08 |
| ORD ID | ord-98d06d6d4bc74f4ab531df5ee852eaa6 |
| Source note | uspto-grants-1981_08 |