反应 #8507

反应方程式

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

溶剂

toluene

反应条件

后处理

1. 1
   温度cooled down
2. 2
   其他The aqueous layer was separated
3. 3
   萃取The compound (12) was extracted with ethyl acetate (50 ml)
4. 4
   洗涤the ethyl acetate layer was washed with water (30 ml)
5. 5
   萃取Each aqueous layer was extracted with ethyl acetate (20 ml)
6. 6
   其他The ethyl acetate layer was collected
7. 7
   浓缩concentrated under reduced pressure
8. 8
   其他to yield oily residue
9. 9
   其他for crystallization
10. 10
    过滤filtered
11. 11
    洗涤washed with diisopropyl ether (30 ml)
12. 12
    其他dried

实验过程

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%

来源