HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 22798533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | 11beta-Trimethylsiloxy-17alpha,21-diacetoxy9alphafluoro-5alpha-pregnane3,20-dione | HCID 22798521 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22798533 | HCID 22798533 | — |
Reaction Steps
A mixture of 8.0 g of 11β-trimethylsiloxy-17α,21-diacetoxy9αfluoro-5α-pregnane3,20-dione obtained according to Example 19, 4 g anhydrous potassium acetate and 20 ml of dimethyl formamide was heated for a period of 4 hours at 110° -120° in an atmosphere of nitrogen. The reaction mixture was cooled and poured into 120 ml of water and ice. The mixture was left stirring for 30 minutes, then lft standing for a period of 2 hours, filtered, washed on the filter with abundant water, collected and dried. Trituration of this crude product with acetone/ether gave 11β-trimethylsiloxy-21-acetoxy-9α-fluoro-5α-pregn-16-ene-3,20-dione (compound 44). Yield: 7.0 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04036831 |
| Source dataset | uspto-grants-1977_07 |
| ORD ID | ord-f934e256490847239476e1321b2584ff |
| Source note | uspto-grants-1977_07 |