Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 86630693 | HCID 86630693 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 86630692 | HCID 86630692 | — |
Reaction Steps
A mixture of 29.4 g 2,7-dibromo-5-chloro-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine, 125 mL methanol, 500 mL THF, 12.9 mL glacial acetic acid and 14.7 g of Zn/Cu pair were stirred at 45° C. After 3 and 5 hours additional portions of 7.3 g Zn/Cu pair were added. The mixture was filtered through celite and the filtrate was diluted with water and ethyl acetate. The phases were separated and the water layer was extracted with ethyl acetate. The combined organic layers were washed with saturated Na2CO3 solution, dried over Na2SO4 and the solvent was evaporated. The solid residue was stirred in a mixture of 2-propanol/ethanol (3:1) for 2 h. The crude product was filtered and dried and 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-11aaaa22288d4a2086668d3b609189d9 |
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| Source note | uspto-grants-2015_02 |
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