反应 #2467962

反应方程式

methyl 3-aminothiophene-2-carboxylate

bromine

→

solid

收率 33.3%

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

收率 33.3%

溶剂

acetic acid

acetic acid

反应条件

后处理

1. 1
   workup.ADDITIONThe reaction mixture was poured into ice cold water
2. 2
   萃取extracted with chloroform (3×100 mL)
3. 3
   洗涤The combined organic layer was washed with water, brine
4. 4
   干燥dried over sodium sulfate
5. 5
   过滤The solution was filtered
6. 6
   其他evaporated the solvent
7. 7
   其他The residue was chromatographed over silica gel column

实验过程

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.

来源