تفاعل #8507

معادلة التفاعل

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

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled down
2. 2
   أخرىThe aqueous layer was separated
3. 3
   استخلاصThe compound (12) was extracted with ethyl acetate (50 ml)
4. 4
   غسيلthe ethyl acetate layer was washed with water (30 ml)
5. 5
   استخلاصEach aqueous layer was extracted with ethyl acetate (20 ml)
6. 6
   أخرىThe ethyl acetate layer was collected
7. 7
   تركيزconcentrated under reduced pressure
8. 8
   أخرىto yield oily residue
9. 9
   أخرىfor crystallization
10. 10
    ترشيحfiltered
11. 11
    غسيلwashed with diisopropyl ether (30 ml)
12. 12
    أخرىdried

الإجراء التجريبي

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%

المصدر