HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → 4-(tert-Butyl-dimethyl-silanyloxy)-2-methyl-benzoic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | Ethyl 4-hydroxy-2-methylbenzoate | HCID 13356900 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(tert-Butyl-dimethyl-silanyloxy)-2-methyl-benzoic acid ethyl ester | HCID 67110261 | — |
Reaction Steps
A mixture of 18 g (100 mmol) of 4-hydroxy-2-methyl-benzoic acid ethyl ester (prepared according to Sen, et. al. (1987), Indian J. Chem. Sec B, 26: 679-682), 10.2 g (150 mmol) of imidazole, and 17.2 g (115 mmol) of tert-butyldimethylsilyl chloride in 110 mL of anhydrous DMF was stirred for 24 hours at room temperature. The reaction was diluted with water and extracted with ethyl acetate. The organic fraction was washed with water, 0.1 N HCl, and brine, then dried over anhydrous magnesium sulfate and concentrated to 28.8 g of the title compound; MS (ESI+): m/z 295.5 (M+1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928120B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-35e68f7adae44b7e9b723dbe9e2bc129 |
| Source note | uspto-grants-2011_04 |