HRID334833

反应详情

EQUATION

反应方程式

HRID 334833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2-(2H-Benzotriazol-2-yl)-6-chloromethyl-4-methyl-phenol (1.0 g, 3.2 mmol) is partly solved in dioxane (19 g) at 80° C. and 1-hexanol (6.6 g, 65 mmol) and sodium hydride (0.2 g, 4.3 mmol, 60% in mineral oil) are added subsequently. The orange reaction mixture is stirred at 80° C. for 2 hours 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 1:30) to yield 940 mg of 2-(2H-Benzotriazol-2-yl)-6-hexyloxymethyl-4-methyl-phenol.

WORKUP

后处理

  1. customevaporated to dryness
  2. dissolutionThe residue is dissolved in ethyl acetate
  3. extractionextracted with aqueous citric acid (5%) and brine
  4. dry with materialThe organic layer is dried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe crude product is purified by column chromatography (ethyl acetate/heptane 1:30)