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 are stirred at 45° C. After 3 and 5 hours additional portions of 7.3 g Zn/Cu pair are added. The mixture is filtered through celite and the filtrate is diluted with water and ethyl acetate. The phases are separated and the water layer is extracted with ethyl acetate. The combined organic layers are washed with saturated Na2CO3 solution, dried over Na2SO4 and the solvent is evaporated. The solid residue is stirred in a mixture of 2-propanol/ethanol (3:1) for 2 h. The crude product is filtered and dried and is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08614218B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-cb032be2c1fb4fdaac0dac14253660d1 |
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| Source note | uspto-grants-2013_12 |
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