反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
Dimethylsulfoxide (25 mL) was added to a mixture of 6-(3-methoxypropoxy)-1H-indol-5-ol described in Production Example 32-5 (3.81 g, 17.2 mmol), N-(4-chloropyridin-2-yl)acetamide described in Production Example 1-5 (3.23 g, 18.9 mmol), and potassium tert-butoxide (2.12 g, 18.9 mmol) under nitrogen atmosphere at room temperature. The liquid mixture was stirred at 150° C. for 14 hours. The reaction liquid was cooled to room temperature, and then ethyl acetate and water were added. The organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration and then the filtrate was concentrated under vacuum. The residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=1:1-0:1-ethyl acetate:methanol=49:1) to obtain the title compound (2.83 g, 46%).
WORKUP
后处理
- customThe reaction liquid
- temperaturewas cooled to room temperature
- washThe organic layer was washed with a saturated saline solution
- dry with materialdried over anhydrous sodium sulfate
- customThe drying agent was separated by filtration
- concentrationthe filtrate was concentrated under vacuum
- customThe residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=1:1-0:1-ethyl acetate:methanol=49:1)