HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178428875, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 178428876 | HCID 178428876 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 178428875 | HCID 178428875 | — |
Reaction Steps
At room temperature, 0.17 g (1.50 mmol) of potassium tert-butoxide was added to a solution of 0.23 g (0.51 mmol) of 4-[2-methyl-3-(5-chloromethyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoyl]-5-hydroxy-1-tert-butyl-1H-pyrazole in 2.5 ml of dimethyl sulfoxide, and the mixture was stirred overnight. The mixture was then stirred into 300 ml of 3% strength aqueous hydrochloric acid, the aqueous phase was extracted three times with in each case 200 ml of ethyl acetate and the combined organic phases were washed four times with in each case 50 ml of water, dried over sodium sulfate and concentrated under reduced pressure. This gave 0.12 g (57%) of the title compound in the form of a brown solid of melting point 69-74° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06627581B1 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-5b235736081847eca316f7533a3179ac |
| Source note | uspto-grants-2003_09 |