Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 66941337 | HCID 66941337 | — |
| Reactant | HCID 131728802 | HCID 131728802 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23079212 | HCID 23079212 | 44.3% |
Reaction Steps
The compound (4.56 g) obtained in Example 11-3 was dissolved in THF (136 ml). Then, the solution was added with a 1 mol/l K-Selectride/THF solution (8.76 ml) while being stirred at −78° C., followed by stirring at the same temperature for 1 hour. The reaction solution was added with a saturated aqueous ammonium chloride solution and then subjected to extraction with chloroform. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate, followed by concentration under reduced pressure. The residue was purified through silica gel column chromatography (hexane/diethyl ether), thereby obtaining the subject compound (2.03 g) as a yellow oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07932281B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-e181e0631d5d45b58c53d26fd5e992cf |
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| Source note | uspto-grants-2011_04 |
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