HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → benzyl 3-(4-cyclopropyl-4H-1,2,4-triazol-3-yl)phenylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | Benzyl 3-(1,3,4-oxadiazol-2-yl)phenylcarbamate | HCID 66851996 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | benzyl 3-(4-cyclopropyl-4H-1,2,4-triazol-3-yl)phenylcarbamate | HCID 66851731 | 31% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
A mixture of (3-[1,3,4]Oxadiazol-2-yl-phenyl)-carbamic acid benzyl ester (200 mg, 0.68 mmol), cyclopropylamine (0.5 mL, 7.2 mmol), trifluoroacetic acid (0.05 mL, 0.65 mmol) in anhydrous 1-butanol (3 mL) was heated at 110° C. overnight in a sealed tube. The reaction mixture was cooled to room temperature and the solvent was removed. The residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution, and the aqueous phase was extracted with ethyl acetate. Solvent was removed after drying with sodium sulfate and purified by silica gel chromatography (rf=0.26 in 20:1 ethyl acetate/methanol) to obtain [3-(4-Cyclopropyl-4H-[1,2,4]triazol-3-yl)-phenyl]-carbamic acid benzyl ester as a white powder (70 mg, 31%). M+1=335.1
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067933B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-db629f5b5e984859ac56b6160a2a365c |
| Source note | uspto-grants-2015_06 |