反应详情

4-amino-2,6-dichlorobenzonitrile (1.65 g, 8.82 mmol) was stirred in 7.5 mL of 12M HCl solution. The reaction mixture was cooled with ice-bath. Sodium nitrite (0.6 g, 8.82 mmol) dissolved in 6 mL of water was added drop-wise to the flask under cold condition, followed by the drop-wise addition of cold potassium iodide (5.86 g, 35.3 mmol) solution in water (12 mL). The mixture was allowed to stir at RT for a day. After the completion of the reaction, the mixture was extracted with ethyl acetate, washed with 10% Na2SO3 solution and brine. The organic layer was dried over anhydrous Na2SO4 and evaporated. The solid obtained was washed with heptane-ethyl acetate mixture (5:1) and dried under vacuum. Yield 1.09 g. 1H NMR (400 MHz; d6-DMSO): δ 6.71 (s, 1H), 6.81 (s, 1H).

1. temperatureThe reaction mixture was cooled with ice-bath
2. additionwas added drop-wise to the flask under cold condition
3. customAfter the completion of the reaction
4. extractionthe mixture was extracted with ethyl acetate
5. washwashed with 10% Na2SO3 solution and brine
6. dry with materialThe organic layer was dried over anhydrous Na2SO4
7. customevaporated
8. customThe solid obtained
9. washwas washed with heptane-ethyl acetate mixture (5:1)
10. customdried under vacuum