HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 90419088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | HCID 90419163 | HCID 90419163 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 90419088 | HCID 90419088 | — |
Reaction Steps
To a solution of tert-butyl-4-acetoxy-4-(but-3-en-1-yl)piperidine-1-carboxylate (1 g, 3.36 mmol) in DMF (6 mL) and H2O (2 mL) was added CuCl (0.77 g, 7.73 mmol) and PdCl2 (0.16 g, 0.91 mmol) and the resulting suspension was stirred under an oxygen atmosphere at room temperature for 24 h. The insoluble materials were removed by filtration, and washed with ethyl acetate. The filtrate was dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel to give 16D (540 mg) as a colorless oil. 1H NMR (CHLOROFORM-d) δ: 3.84 (br. s., 2H), 2.97 (t, J=12.1 Hz, 2H), 2.38-2.47 (m, 2H), 2.17-2.24 (m, 2H), 2.15 (s, 3H), 2.04 (s, 3H), 1.39-1.51 (m, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108921B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-67fae75a567d4ac4b0aafd14577b330f |
| Source note | uspto-grants-2015_08 |