HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → HCID 67609918, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Chlorotriethylsilane | HCID 13819 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Vitamin D3 | HCID 5280795 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67609918 | HCID 67609918 | 87.1% |
Reaction Steps
Commercially available 7-dehydrocholesterol (10.6 g, 27.6 mmol) was dissolved in dichloromethane (90 mL), and then imidazole (3.75 g, 55.1 mmol) and chlorotriethylsilane (6.94 mL, 41.3 mmol) were added at room temperature, followed by stirring for 12 hours. A saturated aqueous ammonium chloride solution was added to the reaction mixture, followed by extraction with chloroform twice. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to yield a residue. The residue was purified by silica gel column chromatography to obtain the title compound (12.0 g, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952003B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-6dc86b002429403a83bbefc28fae957e |
| Source note | uspto-grants-2015_02 |