反应 #42385

反应方程式

sodium bicarbonate

methyl 5-(hydroxymethyl)thiophene-2-carboxylate

phosphorus tribromide

→

title compound

Methyl 5-(bromomethyl)thiophene-2-carboxylate

溶剂

methylene chloride

反应条件

后处理

1. 1
   其他the phases are separated
2. 2
   洗涤The organic phase is washed with water
3. 3
   干燥dried (sodium sulfate)
4. 4
   过滤filtered
5. 5
   浓缩concentrated under reduced pressure

实验过程

To an ice-cold solution of methyl 5-(hydroxymethyl)thiophene-2-carboxylate (375 mg, 2.17 mmol) in methylene chloride (9.0 mL) is added phosphorus tribromide (100 μL, 1.08 mmol) and the reaction mixture is stirred at 0° C. for 0.5 h. Saturated sodium bicarbonate (10 mL) is carefully added to the reaction mixture and the phases are separated. The organic phase is washed with water, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield the title compound in pure form. ESI MS m/z 235 [M+H]+.

来源