HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 178437843, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 21846078 | HCID 21846078 | — |
| Reactant | 5-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide | HCID 22449352 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178437843 | HCID 178437843 | 45% |
Reaction Steps
A mixture of 3-(1-methyl-3-hexahydroazepinyloxy)benzaldehyde (0.79 g, 3.4 mol), 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (0.5 g, 2.2 mmol), methanesulfonic acid (0.25 ml) and xylenes (25 ml) was refluxed overnight. The solvent was stripped, the residue was dissolved in CH2Cl2 and purified by column chromatography on silica gel eluting with ether, then acetone, then 0.5% Et3N/acetone to afford 0.43 g (45%) of 1-cyclopentyl-3-ethyl-6-[3-(1-methyl-3-hexahydroazepinyloxy)phenyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 195-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05958929 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-0ebed79c3e19491192591614d9036e67 |
| Source note | uspto-grants-1999_09 |