반응 #2467962

반응 방정식

methyl 3-aminothiophene-2-carboxylate

bromine

→

solid

수율 33.3%

Methyl 3-amino-4-bromothiophene-2-carboxylate

수율 33.3%

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONThe reaction mixture was poured into ice cold water
2. 2
   추출extracted with chloroform (3×100 mL)
3. 3
   세척The combined organic layer was washed with water, brine
4. 4
   건조dried over sodium sulfate
5. 5
   여과The solution was filtered
6. 6
   기타evaporated the solvent
7. 7
   기타The residue was chromatographed over silica gel column

실험 절차

To a solution of methyl 3-aminothiophene-2-carboxylate (1 g, 6.36 mmol) in acetic acid (10 mL) was added a solution of bromine (0.32 mL, 6.36 mmol) in acetic acid (1 mL) slowly for 5 min at rt and stirred at the same temperature for 16 h. The reaction mixture was poured into ice cold water and extracted with chloroform (3×100 mL). The combined organic layer was washed with water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent. The residue was chromatographed over silica gel column using hexane-EtOAc (95:5) as eluents to give the product as a pale yellow color solid (0.5 g, 33%), mp 58-60° C.

출처