HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → (2-Bromoethoxy)-tert-butyldimethylsilane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | 2-Bromoethanol | HCID 10898 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | (2-Bromoethoxy)-tert-butyldimethylsilane | HCID 3608067 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Combine imidazole (59.9 g, 880 mmol), t-butyldimethylsilyl chloride (60.3 g, 400 mmol), and dimethylformamide (300 mL). Cool to 0° C. in a salt-ice bath. Add dropwise 2-bromoethanol (50.0 g, 400 mmol) at such a rate that the temperature of the reaction mixture does not rise above 0° C. After 2 hours, warm to ambient temperature. After 18 hours, extract the reaction mixture three times with hexane. Combine the hexane layers and extract three times with a saturated aqueous solution of ammonium chloride, three times with a saturated aqueous solution of sodium bicarbonate, and then brine. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06316445B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-1452e6a0175045d1b4bf5f7974ac9750 |
| Source note | uspto-grants-2001_11 |