Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 86630670 | HCID 86630670 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 86630669 | HCID 86630669 | — |
Reaction Steps
6.00 g 5,7-dichloro-2-isopropyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine was dissolved in 360 mL dichloromethane. 360 mL brine, 120 mL ammonia solution 25% w/w and 6.00 g zinc powder were added and the mixture was stirred at room temperature for 3 h. The reaction mixture was filtered through Celite and was washed with dichloromethane and water. The organic phase was separated and the water phase was extracted with dichloromethane. The combined dichloromethane phases were dried over Na2SO4 and evaporated. The crude product contained 5,7-dichloro-2-isopropyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine. The crude product was dissolved again in dichloromethane. 360 mL brine, 120 mL ammonia solution 25% w/w and 6.00 g zinc powder were added and the mixture was stirred at room temperature for 2 h. The reaction mixture was filtered through Celite and washed with dichloromethane and water. The organic phase was separated and the water phase was extracted with dichloromethane. The combined organic layers were dried over sodium sulphate and the solvent was evaporated. The product was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08957064B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-70c34ff9653e4ccd9f2780053d1dd6a5 |
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| Source note | uspto-grants-2015_02 |
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