HRID1505020

反应详情

EQUATION

反应方程式

HRID 1505020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-(4-Octylphenyl)ethanol (53 g) and dichloromethane (500 mL) are charged into a 1 liter three-neck round bottom flask equipped with guard tube and addition funnel. Triethylamine (83.5 g) is added, the mixture is stirred for 30 minutes, then it is cooled to 0° C. Methanesulphonyl chloride (35.2 mL) is added drop-wise at 0° C. and the mass is stirred for 3 hours at room temperature. The mass is diluted with water (700 mL) and the organic layer is separated and the aqueous layer is extracted with dichloromethane (2×250 mL). The combined organic layers is washed with saturated sodium bicarbonate (500 mL) and brine solution (500 mL). The organic layer is separated, dried with sodium sulphate, and concentrated under vacuum to obtain the title compound. Yield: 70 g.

WORKUP

后处理

  1. customequipped with guard tube and addition funnel
  2. stirringthe mass is stirred for 3 hours at room temperature
  3. customthe organic layer is separated
  4. extractionthe aqueous layer is extracted with dichloromethane (2×250 mL)
  5. washThe combined organic layers is washed with saturated sodium bicarbonate (500 mL) and brine solution (500 mL)
  6. customThe organic layer is separated
  7. dry with materialdried with sodium sulphate
  8. concentrationconcentrated under vacuum