HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine | HCID 4184869 | — |
Reaction Steps
To a solution of tert-butyl 4-hydroxypiperidine-1-carboxylate (14.0 g, 70.0 mmol) at 0° C. in triethylamine (9.9 g, 98 mmol) and dichloromethane (100 mL) was added dropwise methanesulfonyl chloride (11.2 g, 98.0 mmol). The reaction was brought to ambient temperature and stirred for 1 h. Then the reaction mixture was quenched with water (50 mL). The aqueous layer was separated and extracted with ethyl acetate (2×50 mL). The combined organic layer was washed with brine (50 mL), and dried over sodium sulfate. The drying agent was removed by filtration and the filtrate was concentrated under reduced pressure to afford 243a, which was used in the next step without further purification (19.5 g, 100%). MS-ESI: [M-t-Bu]+ 224.1
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716274B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-a51aea030bea4f0bae6e57a18ebf0466 |
| Source note | uspto-grants-2014_05 |