反应详情

Iodotrimethylsilane (0.416 mL, 2.92 mmol) was added to a solution of 3-[(5,5-dioxido-3,4-dihydro-2H-1,5-benzoxathiepin-8-yl)oxy]-5-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}-N-(5-methylpyrazin-2-yl)benzamide (150 mg, 0.29 mmol) in acetonitrile (7 mL) and the reaction stirred at RT overnight. Methanol (35 mL) was added, the reaction stirred for 1 hour, then a saturated aqueous solution of sodium thiosulphate (30 mL) was added and the reaction stirred for a further 20 minutes. The mixture was evaporated in vacuo, and the product was extracted away from the inorganic residues by the addition of 20% methanol in DCM (40 mL) with stirring. The organics were reduced in vacuo to a volume of approximately 5 mL. The residue was chromatographed on silica, eluting with 0-20% methanol in DCM, to give the desired compound as a cream solid (79 mg).

1. stirringthe reaction stirred for 1 hour
2. stirringthe reaction stirred for a further 20 minutes
3. customThe mixture was evaporated in vacuo
4. extractionthe product was extracted away from the inorganic residues by the addition of 20% methanol in DCM (40 mL)
5. stirringwith stirring
6. customThe residue was chromatographed on silica
7. washeluting with 0-20% methanol in DCM