반응 #2467991

반응 방정식

nitric acid

sulfuric acid

3-methylthiopheno[2,3-d]1,2,3-triazin-4-one

→

solid

수율 51.1%

3-methyl-6-nitrothiopheno[2,3-d]1,2,3-triazin-4-one

수율 51.1%

반응 조건

후처리

1. 1
   기타was attained to rt
2. 2
   workup.ADDITIONThe mixture was poured into ice cold water
3. 3
   workup.STIRRINGstirred for 15 min
4. 4
   여과The precipitated solid was filtered
5. 5
   기타purified by silica gel column chromatography

실험 절차

To an ice cold (−10° C.) solution of concentrated sulfuric acid (5 mL) was added 3-methylthiopheno[2,3-d]1,2,3-triazin-4-one (0.6 g, 3.6 mmol) for 10 min., nitric acid (0.4 mL, 9 mmol) was added to the above reaction mixture for 5 min and the mixture was attained to rt and stirred for 1 h. The mixture was poured into ice cold water and stirred for 15 min. The precipitated solid was filtered and purified by silica gel column chromatography using hexane-chloroform (1:1) as eluents to give the product as a pale yellow color solid (390 mg, 51%), mp 164-168° C. 1H NMR (400 MHz, DMSO-d6): δ 8.60 (1H, s), 3.99 (3H, s).

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