HRID30101
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
- 150 °C
PROCEDURE
实验过程
A solution of (2,6-Dichloro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone (50.3 mg, 0.178 mmol, Example 4) in 1,4-dioxane (2 mL) was treated with concentrated ammonium hydroxide (0.24 mL, 29.4%) and heated to 150° C. in the microwave for 3 hrs. The resulting mixture was treated with water and ethyl acetate, washed with saturated sodium chloride, dried over sodium sulfate and evaporated in vacuo. The residue was purified on silica gel with hexanes/ethyl acetate to give (2-Amino-6-chloro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone as a off-white solid (23.7 mg, 50.7% yield). HRMS, observed: 262.0502, Calcd for M+: 262.0509.
WORKUP
后处理
- washwashed with saturated sodium chloride
- dry with materialdried over sodium sulfate
- customevaporated in vacuo
- customThe residue was purified on silica gel with hexanes/ethyl acetate