反応 #87536

反応方程式

4-chloro benzonitrile

hydroxyl amine HCl

potassium carbonate

→

desired product

収率 40.4%

4-Chloro-N′-hydroxybenzimidamide

収率 40.4%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The reaction mass was refluxed for 10-12 h
2. 2
   その他Excess of solvent was removed under vacuum
3. 3
   workup.ADDITIONthe residue was diluted with water
4. 4
   その他Precipitate obtained
5. 5
   ろ過was filtered off
6. 6
   その他sucked dried

実験手順

To a solution of 4-chloro benzonitrile (1.000 g, 7.26 mmol) in ethanol (20 mL) was added hydroxyl amine HCl (0.752 g, 10.90 mmol) and potassium carbonate (3.00 g, 21.80 mmol). The reaction mass was refluxed for 10-12 h. Excess of solvent was removed under vacuum and the residue was diluted with water, acidified with dilute HCl. Precipitate obtained was filtered off and sucked dried to afford 0.500 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 5.88 (br s, 2H), 7.42 (d, J=8.1 Hz, 2H), 7.68 (d, J=8.4 Hz, 2H), 9.70 (br s, 1H); MS (m/z): 171.13 (M+H)+.

出典