反应详情

温度

100 °C

To a solution of 6.0 gm of (S)-(−)-4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxy-1-butyl]-3-(hydroxymethyl)-benzonitrile in 30 ml of DMSO at room temperature was added 7.3 gm of anhydrous K2CO3 and 4.04 gm of 2,5-dichloronitrobenzene was added to the above reaction mixture at room temperature and stirred at 100° C. for 15.0 hours. To the above reaction mixture, 120 ml of water was added, and extracted with toluene. The toluene layer was washed with water and 5% sodium hydroxide solution and after acid base treatment yielded an oily product. The oil was dissolved in 16 ml of acetone at 30° C. and 1.9 gm of oxalic acid dihydrate in 8 ml of acetone was added to it, stirred, cooled, filtered and dried at 60° C.

1. additionwas added to the above reaction mixture at room temperature
2. extractionextracted with toluene
3. washThe toluene layer was washed with water and 5% sodium hydroxide solution
4. customafter acid base treatment yielded an oily product
5. stirringstirred
6. temperaturecooled
7. filtrationfiltered
8. customdried at 60° C.