HRID2061157
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
2-(2-Methyl-5-nitrophenyl)acetic acid methyl ester 14 (32 g, 153 mmol) was dissolved in ethanol (750 mL). To this solution was added 10% palladium on carbon (3.2 g). After the mixture was degassed, a balloon filled with hydrogen was fitted. The reaction was stirred at rt for 16 h. After removing the catalyst by filtering through a celite plug and removing the solvent in vacuo, the crude product was purified using flash chromatography (ethyl acetate:petroleum ether=5:1). The product 7 was isolated as a yellow oil. 1H NMR (300 MHz, CDCl3) δ 6.9 (d, J=7.8 Hz), 6.59 (m, 1H), 6.56 (m, 1H), 3.69 (s, 3H).
WORKUP
后处理
- customAfter the mixture was degassed
- additiona balloon filled with hydrogen
- customwas fitted
- customAfter removing the catalyst
- filtrationby filtering through a celite plug
- customremoving the solvent in vacuo
- customthe crude product was purified