HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 118023458, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 118022968 | HCID 118022968 | — |
| Reactant | 3-methyl-1H-pyrazole-4-carbaldehyde | HCID 178434550 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 118023458 | HCID 118023458 | 80% |
Reaction Steps
To a solution of 3-methyl-1H-pyrazole-4-carbaldehyde (273 mg, 2.48 mmol) in anhydrous DMF (5 mL) was added 60% NaH (130 mg, 3.25 mmol) at 0° C. After being stirred for 30 min at room temperature, it was cooled to 0° C. To this, was added intermediate 5 (542 mg, 1.65 mmol) and then stirred for 6 hours at 60° C. Quenching the reaction by addition of ice and 20 mL of water resulted precipitation of brown solids. The resulted solids were collected by filtration, rinsed with water and the dried in vacuo to provide the desired intermediate 6 as a brown solid (424 mg, 80%); MS (ESI) m/z 403 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09212178B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-8c4190f744de473dafbe11228a90b83f |
| Source note | uspto-grants-2015_12 |