HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → trans-Tert-butyl 8-fluoro-5-methyl-6-oxo-1,3a,4,5,6,10b-hexahydrobenzo[c]pyrrolo[3,4-e]azepine-2(3h)-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67166997 | HCID 67166997 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | trans-Tert-butyl 8-fluoro-5-methyl-6-oxo-1,3a,4,5,6,10b-hexahydrobenzo[c]pyrrolo[3,4-e]azepine-2(3h)-carboxylate | HCID 67168442 | — |
Reaction Steps
To a suspension of Example 224A (3.8 g, 11.9 mmol) and iodomethane (2.1 g, 15 mmol) in tetrahydrofuran (15 mL) was added NaH (0.6 g, 60%, 15 mmol) in portions at 0° C. The mixture was stirred for 2 hours and water was then added. The precipitates were collected to afford the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 7.33 (m, 1H), 7.29 (m, 1H), 7.28 (m, 1H), 3.69 (m, 1H), 3.60 (m, 1H), 3.54 (m, 1H), 3.35 (m, 2H), 3.17 (m, 1H), 3.10 (s, 3H), 3.00 (m, 1H), 2.16 (m, 1H), and 1.43 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187483B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-5f87fad28ace47dbaa0add6b0b73bcd7 |
| Source note | uspto-grants-2015_11 |