HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → (S)-[[(Methylsulfonyl)oxy]methyl]piperidine-1-carboxylic Acid tert-Butyl Ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | tert-Butyl (3S)-3-(hydroxymethyl)piperidine-1-carboxylate | HCID 1514448 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | (S)-[[(Methylsulfonyl)oxy]methyl]piperidine-1-carboxylic Acid tert-Butyl Ester | HCID 10469651 | — |
Reaction Steps
To a solution of 7.96 g of {(3S)-1-(tert-butoxycarbonyl)-3-piperidyl}methanol in 150 ml of chloroform, 3.4 ml of methanesulfonyl chloride and 6.7 ml of triethylamine were added under cooling with ice, followed by an hour's stirring at room temperature. The reaction liquid was distilled off under reduced pressure, diluted with ethyl acetate and saturated aqueous sodium bicarbonate solution was added, followed by 1.5 hours' stirring. Thereafter the reaction liquid was successively washed with water and saturated brine and dried over anhydrous magnesium sulfate. Distilling the solvent off, 10.50 g of the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06809108B1 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-7e0619a2470341088e3a032072c06b34 |
| Source note | uspto-grants-2004_10 |