HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 89649349, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 131735926 | HCID 131735926 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 89649349 | HCID 89649349 | 96.7% |
Reaction Steps
A solution of tert-butyl (2R,5R)-2-[4-(5-ethoxy-2-fluoro-phenyl)-3-methyl-2-pyridyl]-7-methyl-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate (which may be prepared as described in Description 100)(74.2 mg, 0.1500 mmol) in 4M HCl in dioxane (0.38 mL, 1.53 mmol) was stirred for 2 hours. The reaction was then concentrated in vacuo. The residue was loaded onto an SCX cartridge which was eluted with MeOH and 0.5 M methanolic ammonia. The basic fractions were combined and concentrated in vacuo to give (2R,5R)-2-[4-(5-ethoxy-2-fluoro-phenyl)-3-methyl-2-pyridyl]-7-methyl-1,7-diazaspiro[4.4]nonan-6-one (55.6 mg, 0.1450 mmol, 94.524% yield) as a colourless oil (5182RTS331-A1, >95% pure);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376436B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-7c76fe9359d842d1b1807346344571db |
| Source note | uspto-grants-2016_06 |