反应详情

A CH2Cl2 solution (20 mL) of 7-7 (44 mg, 0.074 mmol) and TFA (4 mL) was stirred under ambient conditions for 5 h and then concentrated. The residue was azeotroped with toluene (3×25 mL) to give a solid which was purified by HPLC using a VYDAC C18 semiprep column with gradient elution [95:5 (99.9:0.1 H2O/TFA)/(99.9:0.1 CH3CN/TFA)→50:50 (99.9:1 H2O/TFA) (99.9:1 CH3CN/TFA) 60 min] to provide 7-8 as a colorless solid.

1. concentrationconcentrated
2. customThe residue was azeotroped with toluene (3×25 mL)
3. customto give a solid which
4. customwas purified by HPLC
5. washwith gradient elution [95:5 (99.9:0.1 H2O/TFA)/(99.9:0.1 CH3CN/TFA)→50