HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 86733284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 86733129 | HCID 86733129 | — |
| Catalyst | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86733284 | HCID 86733284 | — |
Reaction Steps
A solution of 3α-hydroxy-2β-methoxy-5α-pregnane-11,20-dione (2g.) in methanol (15 ml.) was treated with hydrobromic acid in glacial acetic acid (3 drops). The mixture was stirred at room temperature and bromine (530 mg.) in methanol (1.45 ml.) was added dropwise over a period of 30 minutes. The mixture was stirred for a further 30 minutes and poured into water, stirred, filtered, washed with water and dried. Purification by preparative tlc, followed by crystallisation from ethyl acetate and petrol gave the title compound (250mg) as colourless plates; m.p. 185°-188° [α]D + 104°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03952031 |
| Source dataset | uspto-grants-1976_04 |
| ORD ID | ord-27e6b68f01004539b4630b7ccafb4a10 |
| Source note | uspto-grants-1976_04 |