HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 131735328, compound → HCID 90307385, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 131735328 | HCID 131735328 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 90307385 | HCID 90307385 | 98.1% |
Reaction Steps
A solution of tert-butyl ((4aR,6R,11bR)-3,3,6,11b-tetramethyl-10-nitro-4,4-dioxido-4a,5,6,11b-tetrahydro-3H-benzo[6,7]oxepino[4,5-b][1,4]thiazin-2-yl)carbamate (50 mg, 0.107 mmol) in THF (1 ml) was hydrogenated under hydrogen balloon in the presence of palladium 10 wt. % on activated carbon (34.1 mg, 0.032 mmol) for 1.5 h. The mixture was filtered through the plug of Celite, filter cake was washed with ethyl acetate. The combined filtrate was concentrated to afford crude tert-butyl ((4aR,6R,11bR)-10-amino-3,3,6,11b-tetramethyl-4,4-dioxido-4a,5,6,11b-tetrahydro-3H-benzo[6,7]oxepino[4,5-b][1,4]thiazin-2-yl)carbamate (46 mg, 0.105 mmol, 98% yield) which was used without further purification. MS m/z=438.3 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309263B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-5c8f879617074ec7b192e0a9e7f1e8d8 |
| Source note | uspto-grants-2016_04 |