Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 135671368 | HCID 135671368 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 135671385 | HCID 135671385 | — |
Reaction Steps
To a 5.0 g portion of 7-(3-fluorophenyl)-4,5-dihydropyrazolo[1,5-a]pyrimidine-3-carbonitrile (prepared as described in Ex. 23) in 50 ml of trifluoroacetic acid, stirred under nitrogen and heated to 60° C. was added 7.2 ml of triethylsilane. Heating was continued for 4 hours, then the mixture was stirred at room temperature for 16 hours. The mixture was carefully poured into an ice cooled beaker containing 150 ml of water and 40 g of potassium hydroxide. The precipitate formed was collected, washed with water and dried. The solid was dissolved in dichloromethane and filtered through hydrous magnesium silicate. Evaporation of the filtrate gave a white solid. Recrystallization from isopropyl alcohol gave the desired product, mp 146°-148° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04847256 |
|---|
| Source dataset | uspto-grants-1989_07 |
|---|
| ORD ID | ord-d4b85ee0273844dcb73ba662e6e3f318 |
|---|
| Source note | uspto-grants-1989_07 |
|---|