反应详情

A solution of 4′-chloropropiophenone (5 g) in MeOH (20 ml) was treated under an argon atmosphere and at r.t. with 7M NH3 in MeOH (33.9 ml). Then, tetraisopropyl orthotitanate (10.54 ml) was added dropwise. The reaction mixture was stirred for 1 hr at r.t. Then, trimethylsilyl cyanide (3.72 ml) was added and stirring was continued at r.t. overnight. The reaction mixture was poured in ice and extracted with EtOAc. The organic layer was dried over MgSO4, filtered and concentrated. The crude (RS)-2-amino-2-(4-chloro-phenyl)-butyronitrile (4.95 g) was used in the next reaction step without further purification.

1. stirringstirring
2. waitwas continued at r.t. overnight
3. additionThe reaction mixture was poured in ice
4. extractionextracted with EtOAc
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude (RS)-2-amino-2-(4-chloro-phenyl)-butyronitrile (4.95 g) was used in the next reaction step without further purification