HRID635515

反应详情

EQUATION

反应方程式

HRID 635515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customat room temperature
  2. concentrationThe mixture was concentrated
  3. customto yield a residue which
  4. customwas triturated with ethyl acetate-hexane (1:4)
  5. filtrationfiltered
  6. washwashed with hexane
  7. customdried