反応 #636662

反応方程式

9-bromo-6-chloro-2-(2,6-dibromophenyl)-11H-phenanthro[9,10-d]imidazole

9-bromo-6-chloro-2-(2,6-dibromophenyl)-1H-phenanthro[9,10-d]imidazole

CuCN

DMF

→

2-(9-bromo-6-chloro-1H-phenanthro[9,10-d]imidazol-2-yl)isophthalonitrile

溶媒

brine

ethyl acetate

反応条件

後処理

1. 1
   温度cooled down to room temperature
2. 2
   workup.STIRRINGthe mixture stirred for 30 minutes
3. 3
   洗浄washed with 10% ammonium hydroxide, brine
4. 4
   乾燥dried over sodium sulphate and volatiles
5. 5
   その他were removed under reduced pressure

実験手順

To a solution of 26 g of 9-bromo-6-chloro-2-(2,6-dibromophenyl)-11H-phenanthro[9,10-d]imidazole from Step 4 in 200 mL of dry DMF, was added 14.2 g of CuCN. The reaction was stirred overnight at 85° C., cooled down to room temperature, brine was added and the mixture stirred for 30 minutes. The solution was diluted in ethyl acetate, washed with 10% ammonium hydroxide, brine, dried over sodium sulphate and volatiles were removed under reduced pressure to afford 26 g of 2-(9-bromo-6-chloro-1H-phenanthro[9,10-d]imidazol-2-yl)isophthalonitrile as a solid. 1H NMR (Acetone-d6): 9.19 (s, 1H), 9.02 (s, 1H), 9.71 (bs, 1H), 8.49 (bs, 1H), 8.39 (d, 2H), 8.07 (t, 1H), 7.97 (d, 1H), 8.81 (d, 1H).

出典