反应详情

To a solution of sodium carbonate (89 g, 0.84 mol) in water (830 mL), 2-(carboxymethylamino)benzoic acid of Example 1a (100 g, 0.84 mol) was added in small portions at room temperature under stirring while a clear solution was formed. Acetic anhydride (85.68 g, 0.84 mol) was added dropwise at room temperature under stirring. The reaction mixture was stirred for 30 min, and 37% aqueous hydrochloric acid (140 mL) was added dropwise. The product precipitated slowly. The solid product was filtered off in 12 h, washed with water (3×150 mL) and air-dried to afford 110 g (91%), m.p. 206° C.

1. customwas formed
2. stirringunder stirring
3. stirringThe reaction mixture was stirred for 30 min
4. customThe product precipitated slowly
5. filtrationThe solid product was filtered off in 12 h
6. washwashed with water (3×150 mL)
7. customair-dried
8. customto afford 110 g (91%), m.p. 206° C.