HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 86637728, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Ethyl benzoylacetate | HCID 7170 | — |
| Reactant | Cyclopropanemethanamine | HCID 75646 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86637728 | HCID 86637728 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
Ethyl benzoylacetate (621 mg, 3.23 mmol) and cyclopropylmethylamine (0.34 ml, 3.92 mmol) were dissolved in 1,4-dioxane (1 ml). Para-toluenesulfonic acid (3 crystals, catalytic) was added and the mixture heated under microwave irradiation at 150° C. for 30 min. The crude mixture was poured onto a SiO2 column and purified by flash chromatography (eluted with EtOAc 10 to 35% in hexanes). The title compound was isolated as a yellow solid (309 mg, 44%). HPLC (4 minutes gradient) tR 2.04 min; MS m/z 218.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652044B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-3b23dce3263947a1b28498d69553eb54 |
| Source note | uspto-grants-2010_01 |