HRID1921352

反应详情

EQUATION

反应方程式

HRID 1921352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a mixture of 3-ethyl-2-methoxy-6-methyl-5-[1,3,4]oxadiazol-2-yl-pyridine (10 mg, 0.0457 mmol) and sodium iodide (19 mg, 0.127 mmol) under a nitrogen atmosphere is added anhydrous acetonitrile (2 mL) followed by chlorotrimethylsilane (16.4 μL, 0.131 mmol). The reaction mixture is stirred at 50° C. under nitrogen for 2.5 hr. The reaction mixture is allowed to cool and then quenched with water (0.1 mL). After stirring for 30 min, the mixture is evaporated. The crude residue is purified by flash chromatography on a 2-gram silica gel cartridge by elution with dichloromethane:methanol (49:1). The fraction containing the product is evaporated to give 3-ethyl-6-methyl-5-(1,3,4-oxadiazol-2-yl)-1H-pyridin-2-one (2 mg, 21% yield) as a white solid. LC/MS: RT: 1.98 min, MS: m/e=206 (M+H).

WORKUP

后处理

  1. temperatureto cool
  2. customquenched with water (0.1 mL)
  3. stirringAfter stirring for 30 min
  4. customthe mixture is evaporated
  5. customThe crude residue is purified by flash chromatography on a 2-gram silica gel cartridge by elution with dichloromethane:methanol (49:1)
  6. additionThe fraction containing the product
  7. customis evaporated