HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 88124883, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Hydrazino-delta-2-imidazoline hydrobromide | HCID 3085099 | — |
| Reactant | 3beta,14beta-Dihydroxy-5beta-androstane-17-one | HCID 13117348 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 88124883 | HCID 88124883 | 56.5% |
Reaction Steps
A mixture of 0.60 g of 3β,14β-dihydroxy-5β-androstane-17-one (Lindig C., J. Prakt. Chem., 1983, 325, 587), 1.00 g of 2-hydrazino-2-imidazoline hydrobromide and 1.50 ml of triethylamine in 50 ml of ethanol and 50 mI of water was stirred at reflux for 2 days. After cooling the mixture was added with 1N sodium hydroxide until pH 12.5 was reached. The mixture was evaporated under reduced pressure and the residue was purified by flash-chromatography (SiO2) using chloroform/methanol/28% ammonium hydroxide 88/20/2 as eluant; the fractions containing the title compound were collected and evaporated to dryness. The residue was ground with ethanol/diethyl ether to give 0.43 g of the title compound (I-bo) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05538960 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-c3237d3e139d4599be705e5abd04790b |
| Source note | uspto-grants-1996_07 |