HRID413295
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
In a round-bottomed flask, N-{2-[4-(2-phenyl-thiazol-4-yl)-phenyl]-ethyl}-acetamide (838 mg, 2.60 mmol) was added to 5.0 ml of concentrated HCl and the resulting solution was heated to about 120° C. for about sixteen hours. The solution was then cooled to about 0° C., brought to pH 12 with 5M sodium hydroxide, and extracted with four portions of methylene chloride. The combined organic extracts were then washed with brine, dried over magnesium sulfate, and concentrated in vacua. The crude material was purified by column chromatography (silica gel; methylene chloride to 20% methanol/methylene chloride) to afford the product (617 mg, 85% yield). LRMS ([M+H]+)=281.2.
WORKUP
后处理
- temperatureThe solution was then cooled to about 0° C.
- extractionextracted with four portions of methylene chloride
- washThe combined organic extracts were then washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacua
- customThe crude material was purified by column chromatography (silica gel; methylene chloride to 20% methanol/methylene chloride)