HRID1449565
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 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
- temperaturethe resulting solution was refluxed for 3 hr
- filtrationfiltered
- customto separate the yellow precipitate (0.12 g)
- temperaturein refluxing acetic acid (4.5 mL) for 1 hr
- temperatureAfter cooling to room temperature the reaction mixture
- filtrationwas filtered
- washthe collected solids washed with acetic acid and ethyl acetate
- customAir drying