HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl nitrite → HCID 86692640, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | Ethyl 5-amino-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylate | HCID 722162 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86692640 | HCID 86692640 | 43.8% |
Reaction Steps
tert-Butyl nitrite (154 mg) was added slowly dropwise to a solution of 5-amino-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (300 mg) and N-chlorosuccinimide (200 mg) in dichloromethane (10 ml) and stirred at room temperature for three hours. The reaction solution was concentrated while keeping not dried up, and the residue was purified with silica gel chromatography (ethyl acetate/n-hexane) to give 5-chloro-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (140 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150555B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-17d45f2bf9e4487ca01c558d3046cc21 |
| Source note | uspto-grants-2015_10 |