HRID1014256
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
- 120 °C
PROCEDURE
实验过程
To 1-[2-methyl-5-(methyloxy)-4-nitrophenyl]piperazine (0.300 g, 1.2 mmol) in 10 mL of dioxane was added, ethenyl methyl sulfone (0.32 g, 3 mmol). The mixture was heated to 120° C. 1 hour. The solvent was rotovaped down and the crude product was purified by flash chromatography, followed by a wash of the solids with 30% ether in hexanes to give 1-[2-methyl-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperazine (0.257 g, 0.72 mmol, 60%). 1H NMR (400 MHz, CDCl3) δ ppm 7.80 (s, 1 H), 6.54 (s, 1 H), 3.93 (s, 3 H), 3.18-3.30 (m, 2 H), 2.99-3.10 (m, 9 H), 2.71-2.82 (m, 4 H), 2.23 (s, 3 H).
WORKUP
后处理
- custom1 hour
- customthe crude product was purified by flash chromatography
- washa wash of the solids with 30% ether in hexanes