反応 #8507

反応方程式

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

溶媒

toluene

反応条件

後処理

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

実験手順

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%

出典