反応 #549236

反応方程式

3-(chloromethyl) indole

trichloroacetamidine

→

N-(3-indolylmethyl) trichloroacetamidine

溶媒

ether

ether

反応条件

後処理

1. 1
   温度The mixture is heated
2. 2
   温度at reflux for 3 hours
3. 3
   濃縮concentrated in vacuo to an oil
4. 4
   ろ過filtered
5. 5
   洗浄the chloroform extracts washed first with water
6. 6
   抽出the product extracted with chloroform
7. 7
   洗浄The combined chloroform extracts are washed with water
8. 8
   乾燥dried over magnesium sulfate
9. 9
   ろ過filtered
10. 10
    濃縮concentrated in vacuo

実験手順

A solution of 8.3 g. (0.05 mole) of 3-(chloromethyl) indole in 30 ml. of ether is mixed with a solution of 8.1 g. (0.05 mole) of trichloroacetamidine, also in ether. The mixture is heated at reflux for 3 hours, and concentrated in vacuo to an oil. This is taken up in warm chloroform, filtered, and the chloroform extracts washed first with water and then with dilute hydrochloric acid. The aqueous layers are combined, made basic with a saturated aqueous solution of sodium bicarbonate and the product extracted with chloroform. The combined chloroform extracts are washed with water, dried over magnesium sulfate, filtered and concentrated in vacuo affording N-(3-indolylmethyl) trichloroacetamidine m.p. 135.5 to 138.5 after recrystallization from benzene/hexane.

出典