反应详情

温度

102.5 °C

To a solution of 64 Kg of (S)-(−)-4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxy-1-butyl]-3-(hydroxymethyl)benzonitrile in 300 lit DMSO was added 77.48 Kg of anhydrous K2CO3 and 43.06 Kg of 2,5-dichloronitrobenzene at room temperature and stirred for 16 hours at 100-105° C. To the reaction mixture 3000 ml of water was added at about 30° C. The reaction mixture was 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 510 lit of isopropanol at about 30° C. and 20.4 lit water added, stirred for 10 minutes and 20.8 Kg of oxalic acid dihydrate was added and heated to about 70-75° C., stirred, charcolised, cooled and filtered. The filtrate was cooled to 5-10° C. slowly and the resultant solid was filtered, dried at 60° C. and micronised to get the oxalic acid salt of (S)-(+)-1-[3-(dimethylamino)propyl]-1-(4-fluorophenyl)-1,3-dihydro-5-isobenzofuran carbonitrile.

1. extractionThe reaction mixture was extracted with toluene
2. washthe toluene layer was washed with water and 5% sodium hydroxide solution
3. customafter acid base treatment yielded an oily product
4. additionadded
5. stirringstirred for 10 minutes
6. temperatureheated to about 70-75° C.
7. stirringstirred
8. temperaturecooled
9. filtrationfiltered
10. temperatureThe filtrate was cooled to 5-10° C. slowly
11. filtrationthe resultant solid was filtered
12. customdried at 60° C.