HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 2-(2-Chloro-4-cyano-5-methoxyphenyl)ethyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2-(2-Chloro-4-cyano-5-methoxyphenyl)ethanol | HCID 66644009 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(2-Chloro-4-cyano-5-methoxyphenyl)ethyl methanesulfonate | HCID 86647306 | — |
Reaction Steps
A solution of 2-(2-chloro-4-cyano-5-methoxyphenyl)ethanol (205 mg, 0.969 mmol) DIPEA (0.846 mL, 4.84 mmol) and pyridine (0.0780 mL, 0.969 mmol) in DCM (3 mL) was treated dropwise with mesyl chloride (0.110 mL, 1.42 mmol). The reaction was stirred for 2 hours and was then diluted with DCM and washed twice with aq. citric acid, then washed with brine, and dried over sodium sulfate. Purification of the residue by flash chromatography (20-50% ethyl acetate/hexanes) afforded the title intermediate. 1H-NMR (500 MHz, CDCl3) δ ppm 2.99 (s, 3H), 3.24 (t, J=6.6 Hz, 2H), 3.95 (s, 3H), 4.49 (t, J=6.6 Hz, 2H), 6.962 (s, 1H), 7.563 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673920B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-7e56c3097295436bac7cf197935a44a6 |
| Source note | uspto-grants-2014_03 |