HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 86640601, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 68578477 | HCID 68578477 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86640601 | HCID 86640601 | 91.5% |
Reaction Steps
To a solution of 2-{4-[5-(2-diethylamino-6-methyl-pyridin-4-yl)-[1,2,4]oxadiazol-3-yl]-2-ethyl-6-methyl-phenoxy}-ethanol (850 mg, 2.07 mmol) and DIPEA (401 mg, 3.11 mmol) in DCM (20 mL), methane sulfonylchloride (285 mg, 2.49 mmol) is slowly added. The mixture is stirred at rt for 30 min before it is diluted with EA and washed with sat. aq. NaHCO3-solution. The washing is extracted back three times with EA. The combined org. extracts are dried over MgSO4, filtered, concentrated and dried to give crude methanesulfonic acid 2-{4-[5-(2-diethylamino-6-methyl-pyridin-4-yl)-[1,2,4]oxadiazol-3-yl]-2-ethyl-6-methyl-phenoxy}-ethyl ester (925 mg) as a yellow solid; LC-MS: tR=0.94 min; [M+1]+=489.18.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592460B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-b99b8b7c00f94c549ee488b46f421c8e |
| Source note | uspto-grants-2013_11 |