反应 #63471

反应方程式

2-(3-pyridylcarbonyl)-6-(2-methyl-1,3-dioxolan-2-yl)naphthalene

triethylene glycol

hydrazine

potassium hydroxide

→

2-(3-pyridylmethyl)-6-(2-methyl-1,3dioxolan-2-yl)naphthalene

收率 62.0%

溶剂

water

反应条件

后处理

1. 1
   温度The temperature was then raised to 210° C. for 1 hour
2. 2
   温度The mixture was cooled
3. 3
   萃取extracted with methylene chloride
4. 4
   干燥The organic layer was dried over sodium sulfate
5. 5
   其他the solvent removed under reduced pressure
6. 6
   其他the residue chromatographed on silica gel

实验过程

A mixture of 270 mg of 2-(3-pyridylcarbonyl)-6-(2-methyl-1,3-dioxolan-2-yl)naphthalene, 7 ml of triethylene glycol, 1 ml of anhydrous hydrazine and 500 mg of potassium hydroxide were heated at 160° C. for 30 minutes. The temperature was then raised to 210° C. for 1 hour. The mixture was cooled, poured into water and extracted with methylene chloride. The organic layer was dried over sodium sulfate, the solvent removed under reduced pressure and the residue chromatographed on silica gel to give 160 mg of 2-(3-pyridylmethyl)-6-(2-methyl-1,3dioxolan-2-yl)naphthalene as an oil.

来源