Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Toluene-4-sulfonic Acid 7-(2-Fluorophenyl)pyrazolo[1,5-d][1,2,4]triazin-2-yl Ester | HCID 87798670 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178515394 | HCID 178515394 | 83% |
Reaction Steps
To a stirred solution of toluene-4-sulfonic acid 7-(2-fluorophenyl)pyrazolo[1,5-d][1,2,4]triazin-2-yl ester (82.0 mg, 0.213 mmol) in 1,4-dioxane (4 ml) and water (0.8 ml) was added aqueous 4 N NaOH solution (0.270 ml, 1.08 mmol). The solution was heated at 60° C. for 3 h, then the solvents were removed in vacuo. The residue was dissolved in water (10 ml) and washed with ethyl acetate (10 ml). The aqueous layer was acidified to pH<3 and extracted with dichloromethane (6×25 ml). The combined organic extracts were dried (Na2SO4) and evaporated in vacuo to leave 40.7 mg (83%) of the title compound; 1H NMR (360 MHz, d6-DMSO) δ 6.34 (1H, s), 7.42-7.48 (2H, m), 7.71 (1H, m), 7.79 (1H, td, J 7.2 and 1.7 Hz), 9.40 (1H, s), 11.74 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06476030B1 |
|---|
| Source dataset | uspto-grants-2002_11 |
|---|
| ORD ID | ord-d9dba32cd17142ef9b9653f66da2609e |
|---|
| Source note | uspto-grants-2002_11 |
|---|