反应详情

To a solution of N2-(2-amino-4,6-dimethylphenyl)-N1,N1-dimethylglycinamide from Step B (930 mg, 4.20 mmol) in CH3CN (20 mL) at 0° C. was added triphosgene (1.25 g, 4.20 mmol). The reaction mixture was stirred for 1 h, then quenched with H2O (50 mL) and extracted with CH2Cl2 (3×50 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of CH2Cl2:MeOH—100:0 to 95:5, to give the title compound. MS: m/z=248 (M+1).

1. customquenched with H2O (50 mL)
2. extractionextracted with CH2Cl2 (3×50 mL)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by silica gel chromatography
7. washeluting with a gradient of CH2Cl2