反应详情

A solution of 2-(4-(3-amino-6-methyl-quinolin-4-ylamino)phenyl)-2-methylpropanenitrile (Compound of Preparation J, 190 mg, 0.6025 mmol) and triethylamine (0.12 ml, 0.901 mmol) in CH2Cl2 (10 mL) was added over 40 min to a solution of triphosgene (195 mg, 0.6139 mmol) in 5 mL of CH2Cl2 at 0° C. The reaction mixture was stirred for 20 min at this temperature then was quenched with saturated aqueous NaHCO3, stirred for 5 min and extracted with CH2Cl2. The organic layer was dried over Na2SO4, filtered and evaporated in vacuo to obtain the title compound as brown solid. Yield: 145 mg (70%); 1H NMR (DMSO-d6, 300 MHz): δ 11.641 (s, 1H), 8.678 (s, 1H), 7.864-7.892 (d, 1H, J=8.4 Hz), 7.782-7.810 (d, 2H, J=8.4 Hz), 7.629-7.657 (d, 2H, J=8.4 Hz), 7.342-7.371 (d, 1H, J=8.7 Hz), 6.625 (s, 1H), 2.147 (s, 3H), 1.801 (s, 6H); MS: m/z 343 (M+).

1. customthen was quenched with saturated aqueous NaHCO3
2. stirringstirred for 5 min
3. extractionextracted with CH2Cl2
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated in vacuo