HRID2110403
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
- 90 °C
PROCEDURE
实验过程
Benzenesulfonamide (157 mg, 1.00 mmol) was added to a 10% aqueous solution of sodium hydroxide (0.40 mL, 4.0 mmol). A solution of compound 24A (280 mg, 1.00 mmol) in acetone (1 mL) was then added. The reaction mixture was heated at 90° C. for 8 h then cooled to room temperature. Ice was added and the mixture was extracted with CH2Cl2. The combined organic layers were washed with water, dried and concentrated under reduced pressure. Purification by flash chromatography on silica gel, eluting with CH2Cl2 gave 60 mg (0.23 mmol, 23%) of compound 24B as yellow oil.
WORKUP
后处理
- temperaturethen cooled to room temperature
- additionIce was added
- extractionthe mixture was extracted with CH2Cl2
- washThe combined organic layers were washed with water
- customdried
- concentrationconcentrated under reduced pressure
- customPurification by flash chromatography on silica gel
- washeluting with CH2Cl2