HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 1alpha,3beta-bis(tert-Butyldimethylsilyloxy)-20(S) {(Z)-4-methyl-4-triethylsilyloxy-2-pentenylthio}pregna-5,7,16-triene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1alpha,3beta-bis(tert-butyldimethylsilyloxy)-20(S)-phenoxycarbonylthiopregna-5,7,16-triene | HCID 12019511 | — |
| Reactant | (Z)-1-bromo-4-methyl-4-triethylsilyloxy-2-pentene | HCID 86584697 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1alpha,3beta-bis(tert-Butyldimethylsilyloxy)-20(S) {(Z)-4-methyl-4-triethylsilyloxy-2-pentenylthio}pregna-5,7,16-triene | HCID 70009024 | 64.3% |
Reaction Steps
Under the same conditions as in Example 3, 1α,3β-bis(tert-butyldimethylsilyloxy)-20(S)-phenoxycarbonylthiopregna-5,7,16-triene (91.2 mg, 0.131 mmol), (Z)-1-bromo-4-methyl-4-triethylsilyloxy-2-pentene (192 mg, 0.655 mmol), tetrahydrofuran (1.5 ml) and 1M KOH solution in methanol (1.5 ml) were reacted and worked up, and then the residue was purified by preparative thin layer chromatography (0.5 mm×2, hexane:dichloromethane:ethyl acetate=160:40:1, developed once) to give the title compound as a colorless oil (66.3 mg, 64%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326503B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-7293b25623014b0b8280db537b76a14f |
| Source note | uspto-grants-2001_12 |