HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 21696655, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 21696665 | HCID 21696665 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21696655 | HCID 21696655 | 24.5% |
Reaction Steps
To a solution containing 4-amino-6-trifluoromethylpyridine-2-carboxylic acid methyl ester (0.75 g, 3.4 mmol) in 5 mL of CH3CN was added dropwise a solution of sulfuryl chloride (0.27 mL, 3.4 mmol) in 1 mL of CH3CN. After stirring at RT for 1 hr, reaction mixture was added to 50 mL of Et2O and washed with aqueous NaHCO3, dried over MgSO4, filtered and concentrated to give a solid. The crude product was purified by chromatography, eluting with 10% ethyl acetate-hexane to give 200 mg of product as a white solid; mp 131-3° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06297197B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-c978264ac98144848208ae70e0947b21 |
| Source note | uspto-grants-2001_10 |