HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 58964479, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 58964480 | HCID 58964480 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58964479 | HCID 58964479 | 71.3% |
Reaction Steps
A solution of 450 mg (1.43 mmol) of 2-acetylamino-5-[1,2,4]triazol-4-yl-4-trifluoromethyl-benzoic acid methyl ester in 5 ml methanol and 1 ml water is cooled to 0° C. and treated dropwise with 0.6 ml (11.3 mmol) of concentrated H2SO4. The mixture is then heated to reflux for 30 minutes and allowed to cool to room temperature. It is poured onto ice and the resulting mixture extracted with ethyl acetate. The organic phase is dried over Na2SO4, filtered and concentrated in vacuo. The crude product is recrystallized in ethyl acetate/hexane to give 292 mg (71%) of 2-amino-5-[1,2,4]triazol-4-yl-4-trifluoromethyl-benzoic acid methyl ester, m.p. 184-186° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299085B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-83f1b2765e0648cfbc2c99626429151e |
| Source note | uspto-grants-2012_10 |