反应详情

To 1-[4-({(E)-[(tert-butoxycarbonyl)amino][(tert-butoxycarbonyl)imino]methyl}amino)phenyl]-N-methyl-D-prolinamide (Method 58; 1.9 g) was added DCM (60 ml) and TFA (20 ml). The reaction was stirred for 4 hours before removal of the solvent in vacuo. The reaction was basified with 2.0N KOH (20 ml) and extracted with DCM (2×50 ml). Product failed to extract in to DCM, the aqueous was reduced down to 90% of the initial volume and re-extracted with DCM (3×200 ml), dried and solvent removed in vacuo to yield the title compound as a brown solid (0.84 g, 78%). NMR (299.955 MHz) 7.79 (q, 1H), 7.57 (s, 1H), 7.18 (s, 2H), 7.03 (d, 2H), 6.48 (d, 2H), 3.91 (d, 1H), 3.58-3.54 (m, 1H), 3.17 (q, 1H), 2.56 (d, 3H), 2.19-2.09 (m, 2H), 2.01-1.89 (m, 2H); m/z 261.

1. extractionextracted with DCM (2×50 ml)
2. extractionto extract in to DCM
3. extractionre-extracted with DCM (3×200 ml)
4. customdried
5. customsolvent removed in vacuo