反应详情

Me3SiCl (2.3 mL, 18 mmol) is added to 4-chloroaniline (4.6 g, 36 mmol) in Et2O (50 mL) at room temperature with stirring during 20 min. Following an additional 30 min Stirring 7c (4.05 g, purity 90%, 22 mmol) in Et2O (30 mL) is slowly (1 h) added. The stirring is continued overnight. The precipitate is filtered off and the filtrate extracted with ice-cold 0.1N HCl (50 mL), H2O (3×50 mL), dried (MgSO4) and evaporated. The residue (4.9 g) is extracted with hexane (50 mL) to leave 3.3 g (71%) of the title compound, mp 90°-91° C.

1. waitFollowing an additional 30 min
2. custom(1 h)
3. additionadded
4. waitThe stirring is continued overnight
5. filtrationThe precipitate is filtered off
6. extractionthe filtrate extracted with ice-cold 0.1N HCl (50 mL), H2O (3×50 mL)
7. dry with materialdried (MgSO4)
8. customevaporated
9. extractionThe residue (4.9 g) is extracted with hexane (50 mL)