反应详情

温度

0 °C

To a suspension of 4-methyl-3-(methyloxy)aniline (Reference Intermediate R1, 1.86 g) in water (100 mL)/H2SO4 (30 mL, 563 mmol) at 0° C. a solution of sodium nitrite (1.029 g, 14.91 mmol) in water (10 mL) was slowly added and the reaction mixture was stirred for 30 minutes at 0° C. The reaction mixture was slowly added to a solution of H2SO4 98% (20 mL) in Water (80 mL) pre-heated at 90° C. and stirred at this temperature for 1 h. After cooling the mixture was extracted with Et2O (2×200 mL), the organic layer was dried on sodium sulphate, filtered and evaporated to afford the title compound (1.86 g) as a red/brown oil.

1. additionwas slowly added
2. temperaturepre-heated at 90° C.
3. stirringstirred at this temperature for 1 h
4. temperatureAfter cooling the mixture
5. extractionwas extracted with Et2O (2×200 mL)
6. customthe organic layer was dried on sodium sulphate
7. filtrationfiltered
8. customevaporated