反应详情

[5-chloro-4-(3-chloro-5-cyanophenoxy)-1H-1,2,3-benzotriazol-1-yl]acetic acid (13 mg, 0.036 mmol) (see step 2 in Example 16), piperidine-3-carboxamide (4.6 mg, 0.036 mmol), 3-{[(ethylimino)methylene]amino}-N,N-dimethylpropan-1-aminium chloride (6.9 mg, 0.036 mmol), 3H-[1,2,3]triazolo[4,5-b]pyridin-3-ol (4.9 mg, 0.036 mmol), and triethylamine (0.005 mL, 0.036 mmol) were dissolved in DMF (0.5 mL). After 1 hour, the reaction mixture was diluted with aqueous MeOH (1 mL) and purified by reverse phase chromatography eluting with 30-95% MeCN/H2O+0.1% TFA. Product fractions were lyophilized to yield the title product. 1H NMR (DMSO-d6) δ 7.84 (m, 1H), 7.77 (d, J=4.4 Hz, 1H), 7.76 (s, 2H), 7.58 (m, 1H), 7.51 (m, 1H), 7.44 (m, 1H), 7.36 (m, 1H), 7.02 (m, 1H), 6.84 (m, 1H), 5.97 (m, 2H), 5.93 (m, 1H), 5.87 (m, 0.5H), 5.83 (m, 0.25H), 4.29 (m, 2H), 3.80 (m, 4H), 3.40 (m, 1H), 3.10 (m, 1H), 2.95 (m, 1H), 2.65 (m, 1H), 2.20 (m, 1H), 1.90 (m, 2H), 1.70 (m, 4H), 1.40 (m, 1H). HRMS (M+1)=473.0867.

1. custompurified by reverse phase chromatography
2. washeluting with 30-95% MeCN/H2O+0.1% TFA