تفاعل #656229

معادلة التفاعل

sodium carbonate

2-sulfamoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

potassium hydroxide

hydrochloric acid

→

pure product

المردود 34.9%

2-Sulfamoylthieno[2,3-c]pyridine

المردود 34.9%

المذيبات

water

water

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe product was extracted from this solution with ethyl acetate
2. 2
   تجفيفThe ethyl acetate solution was dried over anhydrous sodium sulfate
3. 3
   ترشيحfiltered through a pad of charcoal
4. 4
   أخرىevaporated
5. 5
   أخرىto give 5.5 g of crude product
6. 6
   أخرىThis material was chromatographed on silica gel
7. 7
   غسيلeluted with ethyl acetate

الإجراء التجريبي

To a solution of potassium ferricyanide (76 g, 0.23 mol) in water (400 ml) was added a solution of potassium hydroxide (68 g, 0.113 mol) in water (150 ml), followed by a suspension of 2-sulfamoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (10.8 g, 49.5 mmol) in water (50 ml). This mixture was warmed at 80° C. for 4-6 hours. This solution was acidified with concentrated hydrochloric acid and then made basic with saturated sodium carbonate solution. The product was extracted from this solution with ethyl acetate. The ethyl acetate solution was dried over anhydrous sodium sulfate, filtered through a pad of charcoal and evaporated to give 5.5 g of crude product. This material was chromatographed on silica gel and eluted with ethyl acetate to give 3.7 g (34.9% yield) of pure product; m.p. 191°-193° C.

المصدر