反应详情

To a solution of 3-bromo-2-methoxyaniline hydrochloride (10 g) prepared as in Example 15, in hydrochloric acid (13.5 mL of concentrated hydrochloric acid in 136.5 mL of water) was added a solution of sodium nitrite (3.47 g in 10 mL of water) at about −5° C. to about 5° C. under stirring. The reaction mixture was stirred for about 1 hour at about −5° C. to about 5° C. Then ethylacetoacetate (6.55 g) was added to the reaction mixture and stirred for about 3 hours at about −5° C. to about 5° C. Sodium bicarbonate and methanol was then added to the reaction mixture. The reaction mixture was stirred at about −5° C. to about 5° C. for about 1 hour. The mixture was filtered to give a solid, which was washed with water and dried at about 50° C. to about 55° C. Yield: 13.3 g

1. stirringThe reaction mixture was stirred for about 1 hour at about −5° C. to about 5° C
2. stirringstirred for about 3 hours at about −5° C. to about 5° C
3. stirringThe reaction mixture was stirred at about −5° C. to about 5° C. for about 1 hour
4. filtrationThe mixture was filtered
5. customto give a solid, which
6. washwas washed with water
7. customdried at about 50° C. to about 55° C