HRID1449565

反应详情

EQUATION

反应方程式

HRID 1449565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of dimethyl 4-aminoquinoline-2,3dicarboxylate (0.15 g, 0.58 mM) in ethanol (4 mL) was added hydrazine hydrate (1.46 g, 29.2 mM) and the resulting solution was refluxed for 3 hr. The reaction mixture was cooled to room temperature and filtered to separate the yellow precipitate (0.12 g). This material was stirred in refluxing acetic acid (4.5 mL) for 1 hr. After cooling to room temperature the reaction mixture was filtered and the collected solids washed with acetic acid and ethyl acetate. Air drying provided the title compound (0.13 g, 68%) as an orange solid, mp >400° C.; MS(CI): 229 (M+H).

WORKUP

后处理

  1. temperaturethe resulting solution was refluxed for 3 hr
  2. filtrationfiltered
  3. customto separate the yellow precipitate (0.12 g)
  4. temperaturein refluxing acetic acid (4.5 mL) for 1 hr
  5. temperatureAfter cooling to room temperature the reaction mixture
  6. filtrationwas filtered
  7. washthe collected solids washed with acetic acid and ethyl acetate
  8. customAir drying