HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanolate methanol → HCID 66760811, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanolate methanol | HCID 23694274 | — |
| Reactant | HCID 66759626 | HCID 66759626 | — |
| Catalyst | Copper bromide (CuBr2) | HCID 24611 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66760811 | HCID 66760811 | 50% |
Reaction Steps
A mixture of 7-bromo-2,2,4,6-tetramethyl-1-benzofuran-3(2H)-one (2.90 g, 10.8 mmol) synthesized in Reference Example 67, copper bromide (1.86 g, 13.0 mmol) and 28% sodium methoxide/methanol solution (60 mL) was stirred under heated reflux for 15 hours. After cooled to room temperature, the reaction solution was poured into water and extracted using ethyl acetate. The extract was washed with saturated saline, and dried using anhydrous magnesium sulfate. After that, the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate 99:1 to 94:6) to give 1.18 g of the title compound (yield: 50%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957069B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-0940796c49cd40f9b9dc66a511fe8ec0 |
| Source note | uspto-grants-2015_02 |