HRID2374477
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 6-amino-1-ethyl-3,3-dimethyl-1,3-dihydro-indol-2-one (5.05 g, 24.72 mmol) in acetic anhydride (80 ml) was stirred at room temperature for 4 h. The mixture was poured onto ice water (150 ml), allowed to warm to room temperature and was stirred again for 2 h. After extraction with ethyl acetate (3×100 ml), the combined organic layers were washed with sat. NaHCO3-solution (3×100 ml), brine (100 ml) and dried over sodium sulfate. After removal of the solvent the crude product was purified by column chromatography on silica gel (ethyl acetate/n-heptane 1:1) yielding 5.6 g (91%) N-(1-ethyl-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-6-yl)-acetamide as light yellow solid.
WORKUP
后处理
- additionThe mixture was poured onto ice water (150 ml)
- extractionAfter extraction with ethyl acetate (3×100 ml)
- washthe combined organic layers were washed with sat. NaHCO3-solution (3×100 ml), brine (100 ml)
- dry with materialdried over sodium sulfate
- customAfter removal of the solvent the crude product
- customwas purified by column chromatography on silica gel (ethyl acetate/n-heptane 1:1)