HRID392849

反应详情

EQUATION

反应方程式

HRID 392849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Bromo-2-methylpropionyl bromide (6.8 mL) was diluted with dichloromethane and added to a solution of triethylamine (7.7 mL) and benzyl alcohol (4.8 mL), while the mixture was cooled in an ice bath and while maintaining an argon atmosphere. The solution was stirred for one hour at 0° C. and then overnight at room temperature. Volatiles were evaporated and the residue was treated with diethylether. The formed salt was removed by filtration and the filtrate was washed with an HCl solution and with water. The ether solution was dried with MgSO4 and concentrated to yield a yellowish liquid. Silica column chromatography using a 2/1 hexane/ethyl acetate mixture as eluent gave a colourless transparent liquid. 1H NMR (400 MHz, CDCl3): δ 7.4 (5H), 5.3 (2H), 2.0 (6H).

WORKUP

后处理

  1. temperaturewas cooled in an ice bath
  2. temperaturewhile maintaining an argon atmosphere
  3. customovernight
  4. customat room temperature
  5. customVolatiles were evaporated
  6. additionthe residue was treated with diethylether
  7. customThe formed salt was removed by filtration
  8. washthe filtrate was washed with an HCl solution and with water
  9. dry with materialThe ether solution was dried with MgSO4
  10. concentrationconcentrated
  11. customto yield a yellowish liquid
  12. customgave a colourless transparent liquid