反应详情

温度

100 °C

To a solution of 10 gm of (RS)-(±)4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxy-1-butyl]-3-(hydroxymethyl)-benzonitrile in 50 ml of dimethylsulfoxide (DMSO) at room temperature was added 12 gm of anhydrous K2CO3 and 6.73 gm of 2,5-dichloronitrobenzene was added to the above reaction mixture at room temperature and stirred at 100° C. for 15 hours. To the reaction mixture, 250 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 40 ml of acetone at 30° C. and 3.4 gm of oxalic acid dihydrate 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.