HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 60142726, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 68153033 | HCID 68153033 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60142726 | HCID 60142726 | 9% |
Reaction Steps
To a mixture of 3-(2-chloro-6-fluorophenyl)-5-(1-(pyridin-3-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)isoxazole-4-carboxylic acid (30 mg, 0.1 mmol) in methanol (1.5 mL) was added thionylchloride (5 μL, 0.1 mmol). The mixture was stirred at room temperature for 60 h and for 5 h at reflux. The mixture was diluted with dichloromethane and washed with water (3×), dried over sodium sulfate, filtered and concentrated under reduced pressure. The product (example IB-67) was purified by pTLC (1:1 EE/PE) to give 3 mg of a white solid (yield 9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354436B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-ec973feca0884621a4446fc3934141e3 |
| Source note | uspto-grants-2013_01 |