HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → Tert-butyl 4-(trifluoromethanesulfonyloxy)-1,2,3,6-tetrahydropyridine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 1,1,1-Trifluoro-N-phenylmethanesulfonamide | HCID 68012 | — |
| Reactant | tert-Butyl 2-oxopiperidine-1-carboxylate | HCID 7577838 | — |
| Reactant | Lithium diisopropylamine | HCID 45051747 | — |
| Product | Tert-butyl 4-(trifluoromethanesulfonyloxy)-1,2,3,6-tetrahydropyridine-1-carboxylate | HCID 10991161 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a −70° C. stirred solution of N-Boc-piperidone (500 mg, 2.5 mmol) in tetrahydrofuran (11 mL) was added lithium diisopropylamine (1.37 mL of a 2 M solution in tetrahydrofuran, 2.75 mmol). The reaction mixture was stirred for 2 h, warmed to 0° C., and N-phenyltriflamide (955 mg, 2.67 mmol) was added. The solution was allowed to warm to room temperature and was stirred for 12 h. The reaction mixture was concentrated under reduced pressure. Purification by flash column chromatography (3:1 hexanes/ethyl acetate) afforded tert-butyl 4-{[(trifluoromethyl)sulfonyl]oxy}-3,6-dihydropyridine-1(2H)-carboxylate (240 mg): 1H NMR (300 MHz, CDCl3) δ 5.77 (s, 1H), 4.05 (m, 2H), 3.63 (m, 2H), 2.45 (m, 2H), 1.48 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176242B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-b6d46ff08eb54cc6a88f9e326d850452 |
| Source note | uspto-grants-2007_02 |