HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyrazole → HCID 20138177, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyrazole | HCID 1048 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 14155950 | HCID 14155950 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 20138177 | HCID 20138177 | — |
Reaction Steps
To a suspension of sodium hydride in dimethylformamide (DMF) is added a solution of pyrazole in DMF. This solution is then added to a solution of 8-(2-chloroethyl)-6,7,8,9-tetrahydro-6-methyl-5H-pyrido[3,2-c]azepin-5-one in DMF. After reaction has occurred, DMF is removed by evaporation (80° C., vacuum pump) and the residue is taken up in chloroform. The chloroform solution is washed with dilute aqueous sodium hydroxide, dried over anhydrous sodium sulfate and concentrated by rotary evaporation (70° C., water aspirator). The residue is subjected to high pressure liquid chromatography using a suitable solvent on a silica gel column.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04746657 |
| Source dataset | uspto-grants-1988_05 |
| ORD ID | ord-82f04645cb0e442eae83b2bbab6cf1e1 |
| Source note | uspto-grants-1988_05 |