HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 17beta-Acetoxy-l-methyl-androsta-1,4-dien-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Carbonate | HCID 11125 | — |
| Reactant | 17beta-Acetoxy-2-iodo-1alpha-methyl-androst-4-en-3-one | HCID 67781852 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 17beta-Acetoxy-l-methyl-androsta-1,4-dien-3-one | HCID 10427505 | — |
Reaction Steps
1.4 g (3 mmol) of 17α-acetoxy-2-iodo-1α-methyl-androst-4-en-3-one of example 11 and 0.443 g (6 mmol) of anhydrous lithium carbonate are stirred in 6 ml of dimethylformamide for 1 hour at 120° C. under nitrogen atmosphere. After cooling, it is added to water and extracted with ethyl acetate. The ethyl acetate solution is dried on sodium sulfate and then concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/hexane as mobile solvent. After concentration by evaporation of the fractions, 0.95 g (92% of theory) of 17β-acetoxy-1-methyl-androsta-1,4-dien-3-one of melting point 173° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05391778 |
| Source dataset | uspto-grants-1995_02 |
| ORD ID | ord-f98ccbc914194730a661b3e8d4e4d3f8 |
| Source note | uspto-grants-1995_02 |