反应详情

温度

4 °C

2-Amino-5-benzenesulfonyl-benzonitrile (0.81 g, 3.15 mmol) in 37% HCl (5 mL) was treated dropwise at 4° C. with NaNO2 (261 mg, 3.78 mmol) in 5 mL of water. After 1.75 hours the suspension was added dropwise to a solution of SnCl2 (4.88 g, 25.21 mmol) in 5 mL of 37% HCl. After stirring at 4° C. for 3 hours the solid was filtered, taken up with water (30 mL) and boiled for 1.5 hours. The hot mixture was filtered and washed thoroughly with boiling water. The filtrate was cooled to 4° C. and treated under stirring with 17% NaOH (approximately 5 mL) dropwise. After overnight cooling in a fridge the solid was filtered and washed with water to neutral pH affording 0.348 g of title compound (40% yield).

1. filtrationwas filtered
2. waitboiled for 1.5 hours
3. filtrationThe hot mixture was filtered
4. washwashed thoroughly with boiling water
5. temperatureThe filtrate was cooled to 4° C.
6. additiontreated
7. stirringunder stirring with 17% NaOH (approximately 5 mL) dropwise
8. temperatureAfter overnight cooling in a fridge the solid
9. filtrationwas filtered
10. washwashed with water to neutral pH