反应详情

温度

50 °C

To a solution of 6′-bromo-5,6,8,9-tetrahydrospiro[benzo[7]annulene-7,2′-inden]-1′(3′H)-one (20 mg, 0.059 mmol) in DCM (2 mL) was added TiCl4 (44.7 mg, 0.235 mmol) dropwise, the mixture was stirred at 50° C. at Ar2 under microwave for 20 minutes, N,N′-methanediylidenebis(1,1,1-trimethylsilanamine) (43.8 mg, 0.235 mmol) was added dropwise. The mixture was stirred at 60° C. at Ar2 under microwave for 10 minutes and repeated the same operation for one time and then poured into ice-water (10 mL). The aqueous layer was extracted with CH2Cl2, which was combined with the organic layer. The organic layer was dried and concentrated to give crude (Z)—N-(5′-bromo-5,6,8,9-tetrahydrospiro[benzo[7]annulene-7,2′-indene]-3′(1′H)-ylidene)cyanamide (20 mg, 4%).

1. stirringThe mixture was stirred at 60° C. at Ar2 under microwave for 10 minutes
2. extractionThe aqueous layer was extracted with CH2Cl2, which
3. customThe organic layer was dried
4. concentrationconcentrated