Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 13714626 | HCID 13714626 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 13714636 | HCID 13714636 | — |
Reaction Steps
To a stirred solution of 2.7 g of 4-aminoandrosta-4,6-dien-3,17-dione in 10.8 ml of dry pyridine are added 5.4 ml of acetic anhydride at room temperature dropwise. After 90 minutes of additional stirring, the reaction mixture is cooled to 0° C. and worked up by the addition of cold water, followed by extraction with ethyl acetate. The organic phase is separated, washed with saturated NaCl aqueous solution, dried over Na2SO4 and evaporated in vacuo to yield a residue which is purified by column chromatography on silica gel. Elution with ethyl acetate:methanol 9:1 yields 2.6 g of the title compound as yellow crystals, m.p. 235°-236° C. (dec.);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04757061 |
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| Source dataset | uspto-grants-1988_07 |
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| ORD ID | ord-9dbe9abcfe524200a9e7f1360412841a |
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| Source note | uspto-grants-1988_07 |
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