HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67431296, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyrazole | HCID 1048 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86634424 | HCID 86634424 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67431296 | HCID 67431296 | — |
Reaction Steps
To a stirred, ice-cooled solution of sodium hydride (45 mg, 1.14 mmol) in anhydrous DMF (10 ml) was added pyrazole (77 mg, 1.14 mmol) and stirring was continued for 30 min. under nitrogen. A solution of compound 11a (0.27 g, 0.95 mmol) in DMF (10 ml) was added slowly and the resultant mixture was stirred at ambient conditions overnight. Water (80 ml) was added and the mixture was extracted with ethyl acetate. The extract was concentrated under reduced pressure and the concentrate was purified by column chromatography on silica gel eluting with a mixture of ethyl acetate and petroleum ether (1:1) to afford 178. (60 mg, 20%). Mp 124-127° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030339B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-8844e27fe7ac41e9aec701578dd435bb |
| Source note | uspto-grants-2011_10 |