反应详情

温度

100 °C

The title compound was prepared according to the method described in Collection Czechoslov. Chem. Commn., vol. 40, p. 719 (1975). To an ice-cold mixture of 2-amino-6-chlorobenzoic acid (10.0 g, 58.3 mmol) and conc. hydrochloric acid (50 mL), was added dropwise a solution of sodium nitrite (4.42 g, 64.1 mmol) in water (10 mL). Furthermore, a solution of potassium iodide (14.5 g, 87.5 mmol) and conc. sulfuric acid (4 mL) in water (30 mL) was added thereto at the same temperature, and the mixture was heated to 100° C. and stirred for 2 hours. The reaction mixture was allowed to cool to room temperature, poured into an aqueous sodium thiosulfate solution, and organic matter was extracted with ethyl acetate. The extract was washed with saturated brine and water and dried over anhydrous sulfuric acid, and the solvent was evaporated under reduced pressure. The resulting crude crystals were collected by filtration, washed with hexane/diethylether, and air dried to give the title compound (12.1 g, 73% yield).

1. customThe title compound was prepared
2. customdescribed in Collection Czechoslov
3. temperatureto cool to room temperature
4. extractionwas extracted with ethyl acetate
5. washThe extract was washed with saturated brine and water
6. dry with materialdried over anhydrous sulfuric acid
7. customthe solvent was evaporated under reduced pressure
8. filtrationThe resulting crude crystals were collected by filtration
9. washwashed with hexane/diethylether, and air
10. customdried