HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86591279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | O-Methylhydroxylamine | HCID 4113 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | (7R,8R,9S,13S,14S)-3,3-dimethoxy-7,13-dimethyl-1,2,4,6,7,8,9,11,12,14,15,16-dodecahydrocyclopenta[a]phenanthren-17-one | HCID 15380148 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86591279 | HCID 86591279 | — |
Reaction Steps
(7α)-3,3-Dimethoxy-7-methylestr-5(10)-en-17-one (100 mg, 0.3 mmol) was added to a solution of methoxylamine.HCl (100 mg, 1.2 mmol) and sodium acetate (123 mg, 1.5 mmol) in 6 mL MeOH. The reaction mixture was stirred for 3 days at room temperature. Water and a solution of saturated sodium hydrogen carbonate was added and extracted with ethyl acetate. The organic layer was washed with brine, dried (Na2SO4) and evaporated to dryness to give the crude (7α)-3,3-dimethoxy-7-methylestr-5(10)-en-17-one O-methyloxime, which was converted into (7α)-3-methylene-7-methylestr-5(10)-en-17-one O-methyloxime according to the methods described above, [α]D +149° (c 0.11 in ethanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06579864B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-0b985c4961754214a6230b067d2db1c3 |
| Source note | uspto-grants-2003_06 |