HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → (+/-)-cis-4-Azidomethyl-3-fluoro-piperidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (Bis(2-methoxyethyl)amino)sulfur trifluoride | HCID 2734690 | — |
| Reactant | (+/-)-trans-4-Azidomethyl-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester | HCID 86657836 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (+/-)-cis-4-Azidomethyl-3-fluoro-piperidine-1-carboxylic acid tert-butyl ester | HCID 86657835 | — |
Reaction Steps
To a stirred solution of (±)-trans-4-azidomethyl-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (1.35 mmol, 350 mg) in dichloromethane (6 mL) was added bis-(2-methoxyethy) aminosulfur trifluoride (1.62 mmol, 358 mg) at −40° C. After stirring the reaction at −40° C. for 3 h, saturated sodium bicarbonate solution (6 mL) was added, and the product was extracted with dichloromethane (6 mL). The organic layer was dried over sodium sulfate and concentrated. The crude product was purified using hexane:ethyl acetate to provide (±)-cis-4-azidomethyl-3-fluoro-piperidine-1-carboxylic acid tert-butyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431575B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-39b7eac1371049a18e766e94603739e2 |
| Source note | uspto-grants-2013_04 |