HRID635515
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a mixture of 10.0 g (66.0 mmol) of 6-methylanthranilic acid in 60 mL of 1,4-dioxane was slowly added 100 mL (193 mmol) of a 1.93 molar solution of phosgene in toluene, at room temperature. The mixture was stirred overnight. The mixture was concentrated to yield a residue which was triturated with ethyl acetate-hexane (1:4), filtered, washed with hexane and dried to afford 11.579 (98.7%) of the 3-methoxyisatoic anhydride as a light brown solid. MS (Cl mode) m/z 160 (M-18,100%),178 (M+H, 95%).
WORKUP
后处理
- customat room temperature
- concentrationThe mixture was concentrated
- customto yield a residue which
- customwas triturated with ethyl acetate-hexane (1:4)
- filtrationfiltered
- washwashed with hexane
- customdried