反应详情

Compound 25.1 (62.2 mg, 0.124 mmol) in CH3CN (1.25 mL, 0.1 M) was treated with 2,6-lutidine (215 μL, 1.85 mmol) and TMSI (176 μL, 1.24 mmol). The mixture was stirred at room temperature for 1 h and the solvent was removed in vacuo. The residue was treated with concentrated NH4OH (2 mL) and the solvent was removed in vacuo (×3). The residue was treated with 1% AcOH (2 mL) and treated to reverse phase HPLC to afford compound 25.2 (19.3 mg, 35% yield) as a white solid: MS (ESI) m/z 448 [M+H]+.

1. customthe solvent was removed in vacuo
2. additionThe residue was treated with concentrated NH4OH (2 mL)
3. customthe solvent was removed in vacuo (×3)
4. additionThe residue was treated with 1% AcOH (2 mL)
5. additiontreated