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
PROCEDURE
实验过程
The compound obtained in the Example 1 (150 mg) was suspended in DMF (30 ml), and 1-hydroxybenzotriazole (74.4 mg), 1-(dimethylaminopropyl)-3-ethylcarbodiimide (106 mg), and a 2 M-ammonia/ethanol solution (0.92 ml) was added to the suspension at room temperature. After the mixture was stirred overnight, chloroform and saturated sodium bicarbonate aqueous solution were added to terminate the reaction. After the aqueous layer was extracted with chloroform twice, the combined organic layer was washed with saturated brine. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure. The resulting residue was purified on column chromatography (MeOH:CHCl3=1:10) to obtain the title compound (128 mg) as a pale yellow solid.
WORKUP
后处理
- customto terminate
- customthe reaction
- extractionAfter the aqueous layer was extracted with chloroform twice
- washthe combined organic layer was washed with saturated brine
- dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe resulting residue was purified on column chromatography (MeOH:CHCl3=1:10)