HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 15296366, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | tert-Butyl 4,4-bis(2-hydroxyethyl)piperidine-1-carboxylate | HCID 15295828 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15296366 | HCID 15296366 | 70% |
Reaction Steps
To a stirred solution of tert-butyl 4,4-bis(2-hydroxyethyl)piperidine-1-carboxylate (500 mg, 1.83 mmol) in DCM (10 ml) were added mesyl chloride (0.33 ml, 4.2 mmol) and TEA (1 ml, 7.32 mmol) at −20° C. and the mixture was stirred for 30 min maintaining the same temperature. TLC revealed completion of the reaction and it was quenched with water and extracted with DCM. The organic phase was washed with brine, dried over Na2SO4 and concentrated to dryness. The crude product was purified by column chromatography (silica (100-200), EtOAc-hexane (30%)) to yield the desired compound. Yield: 70%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08278319B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-a3daa622fbee433aa44d978018aa60b0 |
| Source note | uspto-grants-2012_10 |