HuagongsheHuagongshe Chemistry Print Report · For research reference only
1H-1,2,4-Triazole → HCID 59007752, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1H-1,2,4-Triazole | HCID 9257 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Monosodium phosphate | HCID 23672064 | — |
| Reactant | HCID 57430841 | HCID 57430841 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59007752 | HCID 59007752 | — |
Reaction Steps
0.42 g (11.0 mmol) of 60% sodium hydride in paraffin was added a little at a time to 3.00 g (9.6 mmol) of 3-(2-chloro-6-fluorophenyl)-2,4,6-trichloropyridine and 0.70 g (9.6 mmol) of [1,2,4]triazole dissolved in 30 ml of dimethylformamide. The mixture was stirred at room temperature for 3 d, added to 50 ml of sodium dihydrogenphosphate solution, extracted three times with in each case 50 ml of methyl tert-butyl ether, dried over sodium sulfate and concentrated under reduced pressure. The crude product was chromatographed on silica gel using cyclohexane/ethyl acetate. Yield 1.5 g of a colorless solid of m.p. 210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07695728B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-9ef641533553449093392b6e8d7265c5 |
| Source note | uspto-grants-2010_04 |