HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → (2S,3S,6R,7S,8S)-5-oxo-3-(triethylsilyloxy)-2,4,4,6,8-pentamethyl-7-(2,2,2-trichloroethoxycarbonyloxy)-10-undecenoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | HCID 69507500 | HCID 69507500 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | (2S,3S,6R,7S,8S)-5-oxo-3-(triethylsilyloxy)-2,4,4,6,8-pentamethyl-7-(2,2,2-trichloroethoxycarbonyloxy)-10-undecenoic acid | HCID 86586617 | — |
Reaction Steps
A solution of (4S)-3-[(2S,3S,6R,7S,8S)-5-oxo-3-(triethylsilyloxy)-2,4,4,6,8-pentamethyl-7-(2,2,2-trichloroethoxycarbonyloxy)-10-undecenoyl]-4-benzyloxazolidinone (21.5 g) in 125 mL of 4:1 THF/water is cooled on ice and treated with 10.2 mL of 30% H2O2 followed by a solution of lithium hydroxide (0.96 g) in 50 mL of water. After 1 hour, a solution of sodium sulfite (12.6 g) in 75 mL of water is added, and the mixture is adjusted to pH 3 and concentrated under vacuum. The resulting slurry is extracted with ethyl acetate. The extract is washed with brine, dried over MgSO4, filtered, and evaporated. The product is purified by chromatography on SiO2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176235B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-032f8c5c70834d59beb956241e8e953a |
| Source note | uspto-grants-2007_02 |