HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 19896224, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 53884098 | HCID 53884098 | — |
| Reactant | HCID 67836558 | HCID 67836558 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19896224 | HCID 19896224 | 10.1% |
Reaction Steps
1.27 g of ethyl 3-amino-3-(2-chlorophenyl)-2-propenoate was added dropwise to a 20 ml of dimethylformamide solution of 0.26 g of sodium hydride (purity: 55%). The solution was stirred t room temperature for 15 minutes, then cooled to 0° C. and added with 1.24 g of methyl (5-trifluoromethyl-2-pyridyl)carbamate. The resulting solution was further stirred at 120° C. for 5 hours and then the solvent was distilled away under reduced pressure. The residue was dissolved with 100 ml of water and washed with diethyl ether. The obtained aqueous layer was added into a mixed solution of 20 ml of concentrated hydrochloric acid and 50 g of ice, and the precipitated crystals were filtered out and dried to obtain 0.21 g of the objective compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05116404 |
| Source dataset | uspto-grants-1992_05 |
| ORD ID | ord-e8ff63c6c9eb48bbbda74cdad155ccae |
| Source note | uspto-grants-1992_05 |