HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 117903099, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 117902845 | HCID 117902845 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 117903099 | HCID 117903099 | — |
Reaction Steps
A mixture of 1,2,4,6-tetramethyl-1H,2H,3H-pyrazolo[4,3-c]pyridin-3-one (0.33 g, 1.7 mmol), NBS (0.34 g, 1.9 mmol) and conc. H2SO4 (8 ml) is stirred at RT for 18 h. The mixture is poured onto ice-water. The water phase is made basic with an aqueous solution of sodium hydroxide (1 mol/l) and extracted with DCM. The combined organic layers are dried over MgSO4 and concentrated in vacuo. 7-bromo-1,2,4,6-tetramethyl-1H,2H,3H-pyrazolo[4,3-c]pyridin-3-one is used without further purification. Yield: 0.37 g (80%). HPLC-MS: M+H=270/272; tR=0.77 min (METHOD—1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249151B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-6def95589acf401fada3b08c21c9b10e |
| Source note | uspto-grants-2016_02 |