HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → 2-(3-Iodophenyl)ethyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-(3-Iodophenyl)ethanol | HCID 15169850 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | 2-(3-Iodophenyl)ethyl methanesulfonate | HCID 57444370 | 45% |
Reaction Steps
Methanesulfonyl chloride (1.5 mL, 1.2 eq.) was added dropwise to a stirred solution of 2-(3-iodophenyl)ethanol (3.6 g) in dichloromethane (100 mL) and diisopropylethylamine (3.8 mL, 1.5 equiv.) at 0° C. The solution was warmed to room temperature and stirred for 18 h. The reaction mixture was diluted with aqueous ammonium chloride solution and extracted with dichloromethane. The organic layers were combined, washed with aqueous sodium hydrogencarbonate solution, brine, dried over sodium sulfate and concentrated under reduced pressure. The crude was purified using column chromatography (SiO2 cartridge) using DCM-cyclohexane (70:30) to afford the title compound (3.2 g, 45% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592346B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-006f2a1292694341b4e7eb84af1d1f29 |
| Source note | uspto-grants-2009_09 |