Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 18980983 | HCID 18980983 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18981012 | HCID 18981012 | 42.1% |
Reaction Steps
To 11 g (44 mmole) of crude 2-hydroxymethyl-2-propoxy-4'-chloropropiophenone (Example 96d) in 50 ml of methylene chloride was added 4.5 g (39 mmole) of methanesulfonyl chloride. The mixture was cooled to -40° C. and then 6.0 g (60 mmole) of triethylamine was slowly added. The mixture was allowed to warm to room temperature over 1 hour and was then washed with water, dilute aqueous hydrochloric acid, and brine. It was then dried over anhydrous magnesium sulfate, filtered, concentrated in vacuo, and chromatographed over silica gel using diethyl ether and hexanes to yield 5.5 g of the title compound, an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05798311 |
|---|
| Source dataset | uspto-grants-1998_08 |
|---|
| ORD ID | ord-1c3478f6a8bb433483b2ea576f3e525d |
|---|
| Source note | uspto-grants-1998_08 |
|---|