HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 178432672, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 54699159 | HCID 54699159 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178432672 | HCID 178432672 | 52% |
Reaction Steps
A mixture of 2,4-dimethyl-5-hydroxy-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-8H-pyrido[2,3-d]pyrimidin-7-one (925 mg, 1.92 mmol), methanesulfonic acid (1.84 g, 19.2 mmol), and toluene (10 mL) was heated under reflux for 28 h. 1N KOH (25 mL) was added and the mixture was extracted twice with EtOAC (discarded). The aqueous phase was acidified to pH 4 with 1N HCl and the precipitate (560 mg) was collected by filtration. Recrystallizationfrom EtOH/water gave 424 mg (52%) of product as an off-white solid, mp 278-280 (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05466692 |
| Source dataset | uspto-grants-1995_11 |
| ORD ID | ord-6aeb74f3508246c9b9a3204ce41cbc05 |
| Source note | uspto-grants-1995_11 |