HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86736873, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 86736874 | HCID 86736874 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 86736873 | HCID 86736873 | 68.9% |
Reaction Steps
A solution of 11β-iodoacetoxy-3α-methanesulphonyloxy-5α-pregnan-20-one (22.2 g) in t-butanol (950 ml) containing water (500 ml) was treated with powdered silica gel (44 g) and refluxed with stirring for 75 minutes. The cooled mixture was filtered and the filtrate was evaporated to small bulk and diluted with water. The precipitated solid was collected by filtration and recrystallized from aqueous methanol to afford title compound (12.77 g). A sample recrystallized from acetone-petroleum ether had m.p. 127°-129°, [α]D +100.5°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04192871 |
| Source dataset | uspto-grants-1980_03 |
| ORD ID | ord-1706c84c25e347ccb4b54f70b59dcc0b |
| Source note | uspto-grants-1980_03 |