反应详情

To a magnetically stirred solution of material from Example 2 (2.19 g, 9.04 mmol) in CH2Cl2 (50 mL) is added TFA (25 mL, 324 mmol). The resulting solution is allowed to stir at room temperature for 8 h and then evaporated to dryness under a gentle stream of N2 over 18 h. The resulting tan residue is dissolved in CH2Cl2, sonicated briefly and the solvent is removed in vacuo to give 3.05 g (96%) the title compound as a tan solid as a •1.3 TFA salt by weight. LC/MS (Condition A): ret. T=0.82 min, (M+H)+ 187.00. 1H NMR (500 MHz, DMSO-d6) δ ppm 9.67 (1 H, s), 9.11 (1 H, br. s.), 8.05 (1 H, s), 4.12 (2 H, d, J=5.19 Hz).

1. customevaporated to dryness under a gentle stream of N2 over 18 h
2. dissolutionThe resulting tan residue is dissolved in CH2Cl2
3. customsonicated briefly
4. customthe solvent is removed in vacuo