HuagongsheHuagongshe Chemistry Print Report · For research reference only
Maleic Acid → HCID 68118066, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Maleic Acid | HCID 444266 | — |
| Reactant | HCID 53968227 | HCID 53968227 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68118066 | HCID 68118066 | 67.9% |
Reaction Steps
5-Butyl-3,3a,4,5,6,7-hexahydro-3-phenyl-7-(phenylmethylene)-2-(2,2,2-trifluoroethyl)-2H-pyrazolo[4,3-c]pyridine (5.1 g, see Example 3) and 1.4 g of maleic acid are dissolved in 25 ml of warm acetonitrile and diluted to 400 ml with ether. On seeding and rubbing, the crystalline maleate salt slowly separates. After cooling for about 16 hours, the material is filtered, washed with ether, and dried in vacuo, yielding 4.4 g of material, melting point 150°-155° C (sintering at 130° C). Following crystallization from 15 ml acetonitrile-450 ml ether, the product weighs 3.0 g; melting point 152°-154° C, sintering at 130° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04065617 |
| Source dataset | uspto-grants-1977_12 |
| ORD ID | ord-cb967c830c2b42a492d326fdd8dfe2d0 |
| Source note | uspto-grants-1977_12 |