HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl trifluoroacetate → HCID 21993671, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl trifluoroacetate | HCID 9794 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21993671 | HCID 21993671 | — |
Reaction Steps
To a suspension of tert-butyl 4-aminopiperidine-1-carboxylate (48.7 g, 0.243 mol) and DIPEA (130 mL, 0.749 mol) in DCM (250 mL) was added ethyl trifluoroacetate (35.6 mL, 0.300 mol) dropwise while stirring. After 20 hours, the solution was washed with citric acid solution (200 mL×3, 10% w/v aq) and sodium bicarbonate solution (200 mL×3, conc aq), dried (MgSO4), and filtered through silica (24 g). The silica was washed with DCM and the combined eluant was partially concentrated (100 mL), and used directly in the next step. APCI/MS calcd. for C12H19F3N2O3 296.1. found m/z=294.9 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09161948B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-4b0bf2dbd7c047708fb7576db0af1446 |
| Source note | uspto-grants-2015_10 |