HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 9-Amino-7-methylidenebicyclo[3.3.1]nonan-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | (5,7-Dibromo-adamantan-2-yl)-carbamic acid tert-butyl ester | HCID 16100375 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 9-Amino-7-methylidenebicyclo[3.3.1]nonan-3-one | HCID 67212772 | 163.7% |
Reaction Steps
(First step: Rohde, J. J. et al. Discovery and Metabolic Stabilization of Potent and Selective 2-Amino-N-(adamant-2-yl) Acetamide 11β-Hydroxysteroid Dehydrogenase Type 1 Inhibitors. J. Med. Chem. 2007, 50, 149-64). A solution of 25 (125 mg, 0.305 mmol) in dioxane (0.80 mL) was treated with 2N NaOH (0.70 mL, 1.37 mmol) and irradiated under microwaves (μw, Biotage) for 15 min at 180° C. The dioxane was removed in vacuo. The residue was dissolved in DCM, washed with water, dried (Na2SO4), filtered and concentrated in vacuo to afford 82.5 mg of crude 9-amino-7-methylene-bicyclo[3.3.1]nonan-3-one as a yellow oil, that was used for the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822541B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-d66d71b2214d4d26b6d3016f98981c61 |
| Source note | uspto-grants-2014_09 |