HRID507657

反应详情

EQUATION

反应方程式

HRID 507657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Bromo-1-(5-bromothiophen-2-yl)ethanone (5 g, 17.6 mmol) dissolved in ethanol (100 mL) was treated with an aqueous solution (10 mL) of potassium cyanide (6.19 g, 96.8 mmol) and stirred at ambient temperature overnight. The volatiles were removed in vacuo and crushed iced added to the residue which was acidified to pH 4 with acetic acid. The yellow precipitate that formed was collected by suction filtration and purified by flash chromatography on silica gel using a gradient of 10-30% of ethyl acetate in hexanes to yield a light gray solid (3 g).

WORKUP

后处理

  1. customThe volatiles were removed in vacuo
  2. customcrushed iced
  3. additionadded to the residue which
  4. customThe yellow precipitate that formed
  5. filtrationwas collected by suction filtration
  6. custompurified by flash chromatography on silica gel using a gradient of 10-30% of ethyl acetate in hexanes