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 | 100.2% |
Reaction Steps
To a stirring solution of tert-butyl-4-hydroxy-1-piperidinecarboxylate (10.28 g, 51.08 mmol, Aldrich) and Et3N (14.25 mL, 102.16 mmol, EMD) in CH2Cl2 (300 mL) at room temperature was added methanesulfonyl chloride (4.35 mL, 56.19 mmol, Aldrich) dropwise. The reaction mixture was stirred at room temperature for 4 h and washed with 0.1N HCl aqueous solution, H2O and brine. The organic layer was dried with Na2SO4 and concentrate in vacuo to yield 14.3 g of the crude product as a light orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513424B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-84444bd3f48b438b979daf5901ce7a60 |
| Source note | uspto-grants-2013_08 |