HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22507731, compound → HCID 22507713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22507731 | HCID 22507731 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22507713 | HCID 22507713 | 46% |
Reaction Steps
To a stirred solution of 130 mg (0.29 mmol) (±)-2-(3,6-dihydro-2H-pyran-4-yl)-N-(7-[1,4]dioxan-2-yl-4-methoxy-benzothiazol-2-yl)-isonicotinamide in 10 ml methanol and 10 ml dichloromethane was added a spatula end of 10% palladium on charcoal and the mixture was then stirred for 16 h at room temperature under an atmosphere of hydrogen. The mixture was then filtered, washing with dichloromethane, and the filtrate concentrated in vacuo. Flash chromatography (2/49/49 methanol/dichloromethane/ethyl acetate) followed by trituration in ether afforded 60 mg (46%) (±)-N-(7-[1,4]dioxan-2-yl-4-methoxy-benzothiazol-2-yl)-2-(tetrahydro-pyran-4-yl)-isonicotinamide as a white crystalline solid. ES-MS m/e (%): 456 (M+H+, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06872833B2 |
| Source dataset | uspto-grants-2005_03 |
| ORD ID | ord-dfa4ecbfa98a447bae80077de9dd4c92 |
| Source note | uspto-grants-2005_03 |