反应详情

2-Nitro-4-(trimethylsilylethinyl)aniline (3.96 g; 16.9 mmol; 1 eq.) was dissolved in MeOH (50 ml) and CH2Cl2 (50 ml) and treated with K2CO3 (9.33 g; 67.6 mmol; 4 eq.). After stirring at room temperature for 5 h, the mixture was diluted with water. The organic layer was separated and the aqueous layer was extracted with CH2Cl2 (3×100 ml). The combined organic layers were dried over Na2SO4, evaporated and the residue was purified by flash chromatography on silica using a CHCl3/MeOH gradient. Yield: 2.06 g (75.1%); MS m/z: 163.4 [M+H]+

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with CH2Cl2 (3×100 ml)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. customevaporated
5. customthe residue was purified by flash chromatography on silica using a CHCl3/MeOH gradient