반응 #1869352

반응 방정식

sulfuric acid

5-amino-3-methylisothiazole-4-carbonitrile

ammonia

→

5-Amino-3-methylisothiazole-4-carboxamide

수율 80.0%

반응 조건

후처리

1. 1
   온도The temperature was maintained below 55° C
2. 2
   workup.ADDITIONwas charged to pH 10
3. 3
   온도The mixture was cooled to 20° C., aged overnight
4. 4
   여과filtered
5. 5
   세척The resulting solid was washed with dilute ammonia (3.6 volumes)
6. 6
   기타dried at 40° C.
7. 7
   기타to give a pale brown solid (typical yield 80%)

실험 절차

To a chilled solution of sulfuric acid (7.2 volumes, 12.9 equivs) was charged 5-amino-3-methylisothiazole-4-carbonitrile (method 4) (1.0 equiv). The temperature was maintained below 55° C. The reaction mixture was heated to 70° C. and held for 1 hour until TLC showed disappearance of starting material. The mixture was cooled to 60-65° C. before the ammonia (21 volumes) was charged to pH 10. The mixture was cooled to 20° C., aged overnight and filtered. The resulting solid was washed with dilute ammonia (3.6 volumes) and dried at 40° C. to give a pale brown solid (typical yield 80%).1H NMR (300 MHz, DMSO-d6) δ 2.46(s, 3H), 6.28 (s, 1H).

출처