Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10495279 | HCID 10495279 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10783431 | HCID 10783431 | 83.3% |
Reaction Steps
Sodium hydride (60% purity, 1.0 g, 21.1 mmol) was added to a solution of 2-bromomethyl-5-formylamino-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran (6.0 g, 19.2 mmol) and thiophenol in dimethylformamide (50 ml) and the mixture was stirred at 80° C. for 1 hour under an argon atmosphere. After the reaction mixture was cooled, the product was extracted with ethyl acetate. The extract was washed with water, dried and the solvent was distilled off. The residue was purified by column chromatography on silica gel (isopropyl ether-ethyl acetate, 1:1) and then the purified product was recrystallized from ethanol-isopropyl ether to obtain the desired compound (5.54 g, yield: 83.3% yield), m.p. 130°-131° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05594154 |
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| Source dataset | uspto-grants-1997_01 |
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| ORD ID | ord-f36d117e970847febaeb84f97c5c2e66 |
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| Source note | uspto-grants-1997_01 |
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