HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 86647659, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 49779048 | HCID 49779048 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86647659 | HCID 86647659 | 64.7% |
Reaction Steps
Methanesulfonic acid (309 mg, 3.2 mmol) was added to a solution of compound 4-(3-(4-(imidazo[1,2-a]pyridin-2-ylmethoxy)phenyl)-5,5-dimethyl-4-oxo-4,5-dihydrofuran-2-yl)benzonitrile (1.4 g, 3.2 mmol) in DCM (5 ml) and diethyl ether (30 mL) at RT under an atmosphere of nitrogen. The reaction mixture was stirred at RT for 4 h upon which it was filtered and the solids were washed with 20% DCM in diethyl ether and dried in vacuo to afford 4-(3-(4-(imidazo[1,2-a]pyridin-2-ylmethoxy)phenyl)-5,5-dimethyl-4-oxo-4,5-dihydrofuran-2-yl)benzonitrile methanesulfonate (1.1 g, 64%) as a white solid. 1H NMR: 500 MHz, DMSO-d6: δ 8.55 (d, 1H), 8.0 (s, 1H), 7.55 (Ar, 3H), 7.3-6.85 (Ar, 8H), 5.15 (s, 2H), 2.15 (s, 3H), 1.25 (s, 6H), HPLC: (98.5%, Condition-A).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08343973B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-c21a7bb9c6d24b848f9b4d5e332e5b52 |
| Source note | uspto-grants-2013_01 |