HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 86630688, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 82274691 | HCID 82274691 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 86630688 | HCID 86630688 | — |
Reaction Steps
2.47 g 5,7-dichloro-2-methyl-6-phenylpyrazolo[1,5-a]pyrimidine was dissolved in 80 mL dichloromethane. 80 mL brine, 40 mL ammonia solution 25% w/w and 2.47 g zinc powder were added and the mixture was stirred at room temperature for 2 d. Four additional portions of 4.2 equivalents zinc powder were added over 4 days. The reaction mixture was filtered through Celite and washed with dichloromethane and water. The organic phase was separated and the water phase extracted with dichloromethane. The combined dichloromethane phase was dried over Na2SO4 and the solvent was evaporated. The residue was purified on silica gel (dichloromethane/ethyl acetate) to yield the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957064B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-ecf4d8cf654144019722e630319caceb |
| Source note | uspto-grants-2015_02 |