反応 #348102

反応方程式

sodium hydroxide

1-Chloro-4-nitronaphthalene

5-ethylaminomethyl-1-azabicyclo[3.3.0]octane

sodium iodide

→

desired compound

収率 30.6%

1-[N-(1-Azabicyclo[3.3.0]octan-5-yl )methyl-N-ethylamino]-4-nitronaphthalene

収率 30.6%

溶媒

pyridine

反応条件

後処理

1. 1
   その他to react the mixture in a sealed tube for 20 hours at 190° C
2. 2
   濃縮subsequent to concentration in vacuo
3. 3
   抽出the reaction mixture was extracted by ethyl acetate
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他purified by column chromatography

実験手順

1-Chloro-4-nitronaphthalene (2.00 g, 9.63 mmol), 5-ethylaminomethyl-1-azabicyclo[3.3.0]octane (3.24 g, 19.3 mmol) and sodium iodide (580 mg) were added into anhydrous pyridine (20.0 ml) to react the mixture in a sealed tube for 20 hours at 190° C. After addition of aqueous sodium hydroxide solution subsequent to concentration in vacuo, the reaction mixture was extracted by ethyl acetate, dried over anhydrous sodium sulfate, concentrated in vacuo, and purified by column chromatography to afford the desired compound (1.00 g, 30.6%), as a yellow liquid.

出典