HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 69284672, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 57114671 | HCID 57114671 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69284672 | HCID 69284672 | 96.9% |
Reaction Steps
iv)—A solution of the ketone 5 (140 g) obtained in the previous step in dry tetra-hydrofuran (1400 ml) was added in 30 min. to an ice-cooled suspension of lithium aluminium hydride (35 g) in tetrahydrofuran (1750 ml). After stirring of the mixture for 1 h at room temperature, the reaction was quenched by addition of a saturated aqueous solution of sodium sulfate (152 ml), followed by water (39 ml). Ethyl acetate (1750 ml) was added, and the mixture was filtered over celite. The filtrate was concentrated under reduced pressure to give (3β,20S)-21-[[(1,1-dimethylethyl)dimethylsilyl]oxy]-4,4,20-trimethylpregn-5-en-3-ol (6) (136.3 g), which was used in the following step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06177420B1 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-620745119a5147ca9a5c3b21418cc3fd |
| Source note | uspto-grants-2001_01 |