HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 21-methylene-20(R)-methylpregn-4-en-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Androsta-4,16-dien-3-one | HCID 92979 | — |
| Reactant | Dichloromethane ethylacetate | HCID 21226138 | — |
| Product | 21-methylene-20(R)-methylpregn-4-en-3-one | HCID 15429660 | 48% |
| Product | Estra-1,3,5(10),16-tetraen-6-one-3-yl-acetate | HCID 22873077 | 48% |
Reaction Steps
These syntheses are depicted in FIG. 178. Androsta-4,16-dien-3-one (4) was reduced at -55° with 5 lithium tris (1, 2-dimethylpropyl) hydridoborate in THF (c) as described for the preparation of 2 (FIG. 1). Chromatography on silica gel with CH2Cl2 /ethyl acetate 9:1 gave pure axial alcohol 5 (48% yield) and pure equatorial alcohol 6 (48% yield). Analytical samples were further purified by recrystallization (from PE at -30° for 5, from cyclohexane at RT. for 6).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06066627 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-9ff8d1e9ea5e495bbb0063ce36a02bcc |
| Source note | uspto-grants-2000_05 |