HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178429238, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 68827056 | HCID 68827056 | — |
| Reactant | HCID 178434299 | HCID 178434299 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178429238 | HCID 178429238 | 19% |
Reaction Steps
The product from Step 2 (130 mg, 0.437 mmol, 1.00 equiv), 5-amino-3-methyl indazole (64 mg, 0.437 mmol, 1.0 equiv), and EDC (100 mg, 0.524 mmol, 1.20 equiv) were suspended in 1.0 mL DMF. Et3N (0.073 mL, 0.524 mmol, 1.2 equiv) was added and the solution was stirred at room temperature for 18 hrs. The reaction mixture was diluted with EtOAc and 1N HCl. The phases were separated, and the organic phase was washed twice with 1N HCl, once with satd. NaHCO3, and once with satd. NaCl. The organic phase was dried over Na2SO4, filtered, and concentrated en vacuo. The residue was purified by flash chromatography (0-80% EtOAc in Hexanes) to provide 35 mg (19%) of the title compound as a white solid. MS (ES+) m/e 427 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592357B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-ba4f274cebf2437fb19d34fd9beb9121 |
| Source note | uspto-grants-2009_09 |