HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 68565447, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 68566704 | HCID 68566704 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68565447 | HCID 68565447 | — |
Reaction Steps
(3R,4S)-4-[(3-oxo-3,4-dihydro-2H-benzo-[1,4]thiazin-6-ylmethyl)amino]-3-(trifluoromethyl)piperidine-1-carboxylic acid tert-butyl ester (2e) (1 equiv.) is dissolved in CH2Cl2 and TFA (1:1, v/v). After 2 hrs, the solution is concentrated to dryness under vacuum and the residue is dissolved in 4 M HCl in dioxane. After 30 min, the slurry is triturated with Et2O and filtered. The solid is dissolved in H2O and the solution is made basic with aqueous NaOH. The basic aqueous solution is concentrated under vacuum and the residue is dried under high vacuum. The resulting solid is extracted with CH2Cl2/MeOH (10:1, v/v) and the solution is concentrated. The residue is dried under high vacuum to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07312212B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-1a85e41b2937489181a588a5d22be404 |
| Source note | uspto-grants-2007_12 |