Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Tetrafluoroborate | HCID 26255 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59517061 | HCID 59517061 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68423283 | HCID 68423283 | — |
Reaction Steps
To a suspension of 57.96 g of 2-(4-cyanophenylamino)-2-(2-fluoro-5-methoxy-3-triisopropylsilanyloxyphenyl)thioacetamide in 200 ml of acetonitrile there was added 18.5 g of Me3O+BF4−, and the mixture was stirred at room temperature for 3 hours. After adding 2.1 g of Me3O+BF4− to the reaction mixture, it was further stirred at room temperature for 1 hour. Saturated aqueous sodium hydrogencarbonate was added to the reaction mixture, and extraction was performed with ethyl acetate. After washing the organic layer with saturated brine, it was dried over anhydrous magnesium sulfate. The desiccating agent was filtered off, and the filtrate was concentrated under reduced pressure to give 2-(4-cyanophenylamino)-2-(2-fluoro-5-methoxy-3-triisopropylsilanyloxyphenyl)thioacetimidic acid methyl ester (crude product).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07816522B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-19c0e22fab3d4e60aa70eee2602a6a0a |
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| Source note | uspto-grants-2010_10 |
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