HRID1016449
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
Dissolve 5-amino-4-(4-chloro-2,6-dimethylphenyl)-3-methylpyrazole in 20 mL glacial acetic acid at ambient temperature, and add ethyl acetoacetate (2.0 mL, 1.99 g). Heat to reflux (130° C.) under N2 overnight. Evaporate down to concentrate and add 200 mL Et2O to precipitate out product. Stir at ambient temperature for 1 hour, then filter and wash the resulting white solid (1.25 g) with copious amounts of Et2O. LCMS=302.2 (MH+); 300.2 (M−).
WORKUP
后处理
- temperatureHeat
- customEvaporate down
- concentrationto concentrate
- additionadd 200 mL Et2O
- customto precipitate out product
- filtrationfilter
- washwash the resulting white solid (1.25 g) with copious amounts of Et2O