HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69414776, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | HCID 10453106 | HCID 10453106 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69414776 | HCID 69414776 | 99% |
Reaction Steps
To 0.60 ml of a dimethylsulfoxide solution containing 58.9 mg (0.15 mmol) of 4-(2-acetylaminopyridin-4-yl)-3-(4-fluorophenyl)-1-(1,4,5,6-tetrahydro-6-oxopyridazin-3-yl)-1H-pyrazole obtained in Example 57 was added 15.5 μl (0.18 mmol) of 12N hydrochloric acid at 45° C. over 1 minute, and the mixture was stirred at the same temperature for 15 minutes. Then, 3 ml of ethyl acetate was added to the mixture over 10 minutes, and after gradually cooling the mixture to room temperature, the mixture was further stirred for 30 minutes. Formed crystals were collected by filtration, washed with 3 ml of ethyl acetate, and dried under reduced pressure to obtain 63.5 mg of the title compound as a white powder. (Yield: 99%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07294625B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-83a7b3b2f3684de792f52be5fd5d33fd |
| Source note | uspto-grants-2007_11 |