Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 59140138 | HCID 59140138 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59140115 | HCID 59140115 | 95% |
Reaction Steps
To a solution of 5-fluoro-2-(2-fluoro-4-trimethylsilanyl-phenylamino)-6-formylaminomethyl-nicotinic acid methyl ester (2.6 g, 6.6 mmol) in dichloromethane (65 mL) at −30° C. was added NBS (1.2 g, 6.6 mmol). The reaction mixture was stirred at −30° C. for 1.5 hours, and then concentrated under reduced pressure The resultant residue was taken up in ethyl acetate and this organic solution was washed with a saturated aqueous solution of sodium bicarbonate, followed by brine, dried (Na2SO4), filtered and evaporated in vacuo to afford the title compound as a brown solid (2.49 g, 95%). LCMS (method B): RT=3.79 min, [M+H]+=400/402.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09206174B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-d3b9c660e45b494bb8e715aad3bcd668 |
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| Source note | uspto-grants-2015_12 |
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