HRID631071
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
To a solution of butylbenzene (4.13 g, 30.8 mmol) in CHCl3 (50 mL) was added chlorosulfonic acid (17 mL, 29.8 g, 256 mmol) and the mixture was stirred at rt for 20 h. The mixture was poured on ice (200 mL) and extracted with EtOAc (3×100 mL). The combined extracts were washed with water, a solution of NaHCO3, and water, dried (Na2SO4), and concentrated in vacuo. The yellow oily residue (ca 88% yield) was used without further purification in the next reaction; 1H NMR (300 MHz, CDCl3) δ 0.94 (t, 3H, J=7 Hz), 1.34-1.41 (m, 2H), 1.62-1.67 (m, 2H), 2.73 (t, 2H, J=8 Hz), 7.41 (d, 2H, J=8 Hz), 7.94 (d, 2H, J=8 Hz).
WORKUP
后处理
- additionThe mixture was poured on ice (200 mL)
- extractionextracted with EtOAc (3×100 mL)
- washThe combined extracts were washed with water
- dry with materiala solution of NaHCO3, and water, dried (Na2SO4)
- concentrationconcentrated in vacuo