反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
2-(2H-Benzotriazol-2-yl)-6-chloromethyl-4-(1,1,3,3-tetramethyl-butyl)-phenol (5.0 g, 13.5 mmol) is suspended in isoamyl alcohol (20.0 g, 227 mmol) and stirred at 80° C. for 15 minutes. Sodium hydride (0.2 g, 4.3 mmol, 60% in mineral oil) is added. The orange reaction mixture is stirred at 80° C. for 15 minutes and evaporated to dryness. The residue is dissolved in ethyl acetate and extracted with aqueous citric acid (5%) and brine. The organic layer is dried over sodium sulphate, filtered and evaporated to dryness. The crude product is purified by column chromatography (ethyl acetate/heptane 1:12) to yield 3.7 g of 2-(2H-Benzotriazol-2-yl)-6-(3-methyl-butoxymethyl)-4-(1,1,3,3-tetramethyl-butyl)-phenol.
WORKUP
后处理
- stirringThe orange reaction mixture is stirred at 80° C. for 15 minutes
- customevaporated to dryness
- dissolutionThe residue is dissolved in ethyl acetate
- extractionextracted with aqueous citric acid (5%) and brine
- dry with materialThe organic layer is dried over sodium sulphate
- filtrationfiltered
- customevaporated to dryness
- customThe crude product is purified by column chromatography (ethyl acetate/heptane 1:12)