反応 #6311

反応方程式

2-chloro-3-nitropyridine

potassium isothiocyanate

→

title compound

2-isothiocyanato-3-nitro pyridine

溶媒

acetic acid

反応条件

後処理

1. 1
   温度refluxed for 2 h
2. 2
   温度The reaction mixture was then cooled
3. 3
   洗浄The resulting solid was washed with water
4. 4
   workup.DISSOLUTIONredissolved in ethyl acetate
5. 5
   洗浄washed (4×) with water
6. 6
   workup.ADDITIONThe ethyl acetate solution was then treated with activated carbon
7. 7
   乾燥dried over anhydrous Na2SO4
8. 8
   ろ過filtered
9. 9
   その他evaporated to dryness

実験手順

A 10 g sample of 2-chloro-3-nitropyridine, an 8 g sample of potassium isothiocyanate, and 75 ml of acetic acid were combined and refluxed for 2 h. The reaction mixture was then cooled and poured into 400 ml of ice/H2O. The resulting solid was washed with water, redissolved in ethyl acetate and washed (4×) with water. The ethyl acetate solution was then treated with activated carbon, dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide 3.72 g of the title compound. m.p.=115°-118° C.

出典