HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66759725, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-Butyldimethylsilyl trifluoromethanesulphonate | HCID 123564 | — |
| Reactant | HCID 23114238 | HCID 23114238 | — |
| Reactant | Sodium bicarbonate water | HCID 86585896 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66759725 | HCID 66759725 | 95% |
Reaction Steps
Triethylamine (2.15 g, 21.2 mmol) and tert-butyldimethylsilyl trifluoromethanesulfonate (4.68 g, 17.7 mmol) were sequentially added to a solution of toluene (100 mL) containing 5-bromo-4,6,7-trimethyl-1-benzofuran-3(2H)-one (3.00 g, 11.8 mmol) synthesized in Reference Example 45, and the mixture was stirred at room temperature for 1 hour. The resulting mixture was poured into saturated sodium bicarbonate water, and extraction was performed using ethyl acetate. The extract was washed with saturated saline, and dried using anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was purified by silica gel chromatography (hexane-ethyl acetate 99:1 to 94/6) to give 4.14 g of the title compound (yield: 95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288390B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-062a0fc10173478fbb2e98498165b4bb |
| Source note | uspto-grants-2012_10 |