HRID1743837
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
- 0 °C
PROCEDURE
实验过程
To a solution of 2-(2-chloro-6-nitrophenyl)ethanol (33.0 g, 0.16 mole) in methylene chloride (500 mL) was added triphenylphosphine (43.0 g, 0.16 mole) and the mixture was cooled to 0° C. Carbon tetrabromide (54.4 g, 0.16 mole) in methylene chloride (100 mL) was added dropwise through an addition funnel. The reaction mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue purified by flash column chromatography (silica gel, ethyl acetate:hexanes 1:9) to provide 39.0 g of the title compound as a yellow solid. 1H NMR (CDCl3): 7.70 δ (d, 1H); 7.60 δ (d, 1H); 7.35 δ (t, 1H); 3.60 δ (t, 2H); 3.45 δ (t, 2H).
WORKUP
后处理
- customThe solvent was removed in vacuo
- customthe residue purified by flash column chromatography (silica gel, ethyl acetate:hexanes 1:9)