HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 44467389, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 1-[4-(4-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 736269 | — |
| Reactant | HCID 57990388 | HCID 57990388 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 44467389 | HCID 44467389 | 11.3% |
Reaction Steps
A mixture of tert-butyl (1-(2-(1H-benzo[d][1,2,3]triazol-1-yloxy)-5-carbamoylpyrimidin-4-yl)piperidin-4-yl)methylcarbamate (138 mg, 0.294 mmol), 1-(4-(4-aminophenyl)piperazin-1-yl)ethanone (84 mg, 0.38 mmol) and p-toluenesulfonic acid (56 mg, 0.294 mmol) in dioxane (4 mL) was stirred at 100° C. for 3 h. dioxane was removed in vacuo. The residue was dissolved in CH2C12 (5 mL) and TFA (5 mL). The solution was stirred at room temperature for 30 min. It was then concentrated in vacuo. The residue was purified by HPLC to give the titled compound (15 mg). MS 453.6 (M+H); UV 222.8, 263.8 nm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09139581B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-1c90cb74b8194a8ca2a3e5e0136ae745 |
| Source note | uspto-grants-2015_09 |