HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2Chlor-3-[1-(3-chlor-4,5,6,7-tetrahydropyrazolo-[1,5-a]-pyridin-2-yl)-4-cyan-5-pyrazolyl]-2-methyl-propionic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Methacrylate | HCID 7343 | — |
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | 5-Amino-1-(3-chloro-4,5,6,7-tetrahydropyrazolo[1,5-a]pyridin-2-yl)-1h-pyrazole-4-carbonitrile | HCID 15376433 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2Chlor-3-[1-(3-chlor-4,5,6,7-tetrahydropyrazolo-[1,5-a]-pyridin-2-yl)-4-cyan-5-pyrazolyl]-2-methyl-propionic acid ethyl ester | HCID 57322157 | — |
Reaction Steps
1.6 g (15.5 mmol) tert-butyl nitrite, 20 ml ethyl methacrylate and 1.52 g copper-ll-chloride is added to 20 ml acetonitrile and 2.62 g (10 mmol) 5-amino-1-(3-chlor-4,5,6,7-tetrahydropyrazolo-[1,5-a]-pyridin-2-yl)-4-pyrazol-carbonitrile is added in 3 portions. The mixture is stirred at room temperature for 20 hours, added to 50 ml 2N hydrochloric acid, extracted 3 times with dichloromethane, dried over magnesium sulphate and concentrated. Purification is by column chromatography using a hexane/ethyl acetate mixture.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06057270 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-c70d98158ebb4c2fbdbff97118f3ec35 |
| Source note | uspto-grants-2000_05 |