反应详情

温度

90 °C

2-cyanobenzocycloheptan-1-one (compound Ia) was prepared by dissolving 2-bromobenzocycloheptan-1-one (30.2 g, 0.126 mol) in toluene (150 mL) in a 500 mL round bottom flask equipped with a condenser. NaCN (18.6g, 0.38 mol), water (50 g), and dibenzo-18-crown-6 (0.5 g) were added to the flask. The reaction mixture was stirred vigorously at 90° C. under a static blanket of nitrogen for 15 hours. The reaction mixture was cooled and washed three times with water (70 mL×2+100 mL). The toluene solution was dried over sodium sulfate and filtered. The solvent was evaporated under reduced pressure. The residue was distilled under vacuum to give a yellow liquid (21.1 g, b.p. 158-162° C. at 17 mm Hg). The purity of the liquid was 96% by GC.

1. customequipped with a condenser
2. temperatureThe reaction mixture was cooled
3. washwashed three times with water (70 mL×2+100 mL)
4. dry with materialThe toluene solution was dried over sodium sulfate
5. filtrationfiltered
6. customThe solvent was evaporated under reduced pressure
7. distillationThe residue was distilled under vacuum
8. customto give a yellow liquid (21.1 g, b.p. 158-162° C. at 17 mm Hg)