HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 86668519, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 86668520 | HCID 86668520 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86668519 | HCID 86668519 | 85% |
Reaction Steps
To a solution of 190 mg (0.393 mmol) 3-(2-chloro-6-fluorophenyl)-5-(1-(2-fluorophenyl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)isoxazole-4-carbohydrazide (which was synthesized in analogy to the procedure described for example I-133) in 5.8 ml absolute dioxane, 148 mg (1.885 mmol) acetyl chloride were added. The conversion is complete within minutes. Volatiles were evaporated, residue was re-evaporated with ethanol. Residue was crystallized from EtOAc-heptane to give 175 mg (85%) of compound I-142 as a pale yellow powder. Result of LC/MS MH+: 526.06; 1H-NMR (400 MHz, methanol-d4) δ ppm: 1.98 (3H, s, CH3), 7.25-7.32 (1H, m, CH-arom.), 7.41-7.48 (3H, m, CH-arom.), 7.54-7.61 (1H, m, CH-arom), 7.64-7.74 (1H, m, CH-arom.), 8.63 (1H, s, CH-pyraz.)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354436B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-f8369a32a69d496c9c3eaf3cbc6dbfa5 |
| Source note | uspto-grants-2013_01 |