HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → 2-{[Tert-butyl(dimethyl)silyl]oxy}-3-chloropropyl 4-methylbenzenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3-Chloro-2-hydroxypropyl 4-methylbenzenesulfonate | HCID 12461087 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-{[Tert-butyl(dimethyl)silyl]oxy}-3-chloropropyl 4-methylbenzenesulfonate | HCID 86662971 | 81.5% |
Reaction Steps
To a mixture of 3-chloro-2-hydroxypropyl 4-methylbenzenesulfonate (17.4 g) and imidazole (13.4 g) in DMF (130 mL) was added tert-butyl(chloro)dimethylsilane (14.9 g), and the mixture was stirred for 64 hr. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and the mixture was extracted with hexane. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (20.3 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822699B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-c1b00079bedf4880986324ae8d87e8d5 |
| Source note | uspto-grants-2014_09 |