반응 #8507

반응 방정식

diisopropyl ether

water

compound ( 6 )

2-Benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(pyridin-4-yl)methyl-1H-imidazole

hydrochloric acid

→

compound ( 12 )

2-Hydroxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(pyridin-4-yl)methyl-1H-imidazole

용매

toluene

반응 조건

후처리

1. 1
   온도cooled down
2. 2
   기타The aqueous layer was separated
3. 3
   추출The compound (12) was extracted with ethyl acetate (50 ml)
4. 4
   세척the ethyl acetate layer was washed with water (30 ml)
5. 5
   추출Each aqueous layer was extracted with ethyl acetate (20 ml)
6. 6
   기타The ethyl acetate layer was collected
7. 7
   농축concentrated under reduced pressure
8. 8
   기타to yield oily residue
9. 9
   기타for crystallization
10. 10
    여과filtered
11. 11
    세척washed with diisopropyl ether (30 ml)
12. 12
    기타dried

실험 절차

To the compound (6) was added concentrated aqueous hydrochloric acid (50 ml). The mixture was heated at 90° C. for 2 hours and then cooled down. To the mixture were added water (50 ml) and toluene (20 ml). The aqueous layer was separated and neutralized by 30% aqueous sodium hydroxide. The compound (12) was extracted with ethyl acetate (50 ml), and the ethyl acetate layer was washed with water (30 ml). Each aqueous layer was extracted with ethyl acetate (20 ml). The ethyl acetate layer was collected and concentrated under reduced pressure to yield oily residue. To the oily residue was slowly added diisopropyl ether (50 ml) for crystallization. The obtained slurry was stirred at room temperature for 30 minutes, filtered, washed with diisopropyl ether (30 ml) and dried to yield the compound (12) (10.4 g) as a white crystal. Yield from the compound (22):82%

출처