HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Difluorophenylacetic acid → HCID 86662121, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Difluorophenylacetic acid | HCID 145424 | — |
| Reactant | Thiosemicarbazide | HCID 2723789 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | HCID 178418300 | HCID 178418300 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86662121 | HCID 86662121 | 46.9% |
Reaction Steps
2.5 g of 3,5-difluorophenylacetic acid (14.52 mmol, 1 eq.) are placed in 70 mL of dichloromethane with stirring. 1.46 g of thiosemicarbazide (15.98 mmol, 1.1 eq.), 2.22 g of hydroxybenzotriazole (14.52 mmol, 1 eq.) and 2.78 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (14.52 mmol, 1 eq.) are successively added with continued stirring at room temperature. After 18 hours at room temperature, the dichloromethane is evaporated off. The residue is taken up in ethyl acetate and 1N hydrochloric acid. The precipitate is filtered off and dried to give 1.67 g of [(3,5-difluorophenyl)acetyl]hydrazinecarbothioamide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546391B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-6e3fb33811ae474493a04d01990f39cc |
| Source note | uspto-grants-2013_10 |