HRID334841

反应详情

EQUATION

反应方程式

HRID 334841 的结构方程式

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

  1. stirringThe orange reaction mixture is stirred at 80° C. for 15 minutes
  2. customevaporated to dryness
  3. dissolutionThe residue is dissolved in ethyl acetate
  4. extractionextracted with aqueous citric acid (5%) and brine
  5. dry with materialThe organic layer is dried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe crude product is purified by column chromatography (ethyl acetate/heptane 1:12)