HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53673654, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-Nitrobenzaldehyde | HCID 7449 | — |
| Reactant | HCID 10559247 | HCID 10559247 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 53673654 | HCID 53673654 | 82.9% |
Reaction Steps
A solution containing 12.2 g of 3-nitrobenzaldehyde and 14.3 g of 1-methyl-2-chloroethyl acetoacetate in 80 ml of toluene, maintained at 0°-5° C., was saturated with hydrogen chloride gas. After two days at 20°-25° C., the residual hydrogen chloride was removed by bubbling nitrogen through the solution. The toluene was then evaporated off in vacuo. The residual oil was dissolved in dichloromethane and the solution thus obtained was washed with water until it was neutral. The organic phase which was separated and dried, was then evaporated to dryness under vacuum at 20° C. The residue was crystallized from 200 ml of isopropanol to give 20.70 g of the title compound, melting at 95°-96° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04772621 |
| Source dataset | uspto-grants-1988_09 |
| ORD ID | ord-6b42b4b71ce24831804c7314e9899ae0 |
| Source note | uspto-grants-1988_09 |