反应详情

温度

110 °C

A pressure flask was charged with 3e (30.92 g), glycine (22.52 g), methanol (155 mL), sodium methoxide solution (64.81 g) and sealed (as an alternative, sodium glycinate was used in place of glycine and sodium methoxide). The reaction was heated to about 110° C. until reaction was complete. The mixture was cooled, filtered, washed with methanol, dried under vacuum, dissolved in water and washed with ethyl acetate. The ethyl acetate was removed and to the resulting aqueous layer an acetic acid (18.0 g) solution was added. The suspension was stirred at room temperature, filtered, and the solid washed with water (3×30 mL), cold acetone (5-10° C., 2×20 mL), and dried under vacuum to obtain 2-(4-hydroxy-1-methyl-7-phenoxyisoquinoline-3-carboxamido)acetic acid (Yield: 86.1%, HPLC: 99.8%).

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washwashed with methanol
4. customdried under vacuum
5. dissolutiondissolved in water
6. washwashed with ethyl acetate
7. customThe ethyl acetate was removed and to the resulting aqueous layer an acetic acid (18.0 g) solution
8. additionwas added
9. filtrationfiltered
10. washthe solid washed with water (3×30 mL), cold acetone (5-10° C., 2×20 mL)
11. customdried under vacuum