Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Nitropropane | HCID 398 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 12401525 | HCID 12401525 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 12401526 | HCID 12401526 | — |
Reaction Steps
11.6 g of 2-nitropropane are introduced at about 30° C. into a solution of 2.3 g of sodium in 450 ml of absolute ethanol. The mixture is stirred for a further 1 hour and a solution of 28.8 g of 2-(p-bromomethyl-phenyl)-s-triazolo[1,5-a]pyridine (I) in 290 ml of dimethylformamide is now added. Subsequently, the reaction mixture is warmed to 50° C., then stirred for 20 hours without external warming and finally cooled to -10° C. The product which has precipitated is filtered off, washed with cold methanol and dried. This gives 19.3 g (86.5% of theory) of compound (II) in the form of a pale yellow powder with a melting point of 243° to 244° C. After recrystallising twice from dimethylformamide, 14.67 g (65.7% of theory) of small, virtually colourless, glossy needles with a melting point of 246° to 247° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04113937 |
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| Source dataset | uspto-grants-1978_09 |
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| ORD ID | ord-db9753bbc01042188bf6151703c27a4a |
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| Source note | uspto-grants-1978_09 |
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