反応 #63471

反応方程式

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

収率 62.0%

溶媒

water

反応条件

後処理

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
   抽出extracted with methylene chloride
4. 4
   乾燥The organic layer was dried over sodium sulfate
5. 5
   その他the solvent removed under reduced pressure
6. 6
   その他the residue chromatographed on silica gel

実験手順

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.

出典