HRID2236531

反应详情

EQUATION

反应方程式

HRID 2236531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

An amount of 1.0 g (4.1 mmol) of 4-bromo-2-(diethoxymethyl)furan, is dissolved in ether (15 mL) and cooled to −78° C. To this is added 4.3 mL (6.02 mmol) of sec-butyllithium. After stirring at −78° C. for 30 minutes, triisopropyl borate (1.10 mL, 5.01 mmol) is added dropwise. The mixture is stirred at −78° C. for 1.5 hours and brought to room temperature for 2 hours. The mixture is hydrolyzed with 2N HCl and stirred at room temperature for 1 hour. The ether layer is separated and the water layer is washed once more with ether. The combined ether layers is washed once with brine and dried with sodium sulfate. Evaporated to give 563 mg of the boronic acid as dark oil.

WORKUP

后处理

  1. stirringThe mixture is stirred at −78° C. for 1.5 hours
  2. waitbrought to room temperature for 2 hours
  3. stirringstirred at room temperature for 1 hour
  4. customThe ether layer is separated
  5. washthe water layer is washed once more with ether
  6. washThe combined ether layers is washed once with brine
  7. dry with materialdried with sodium sulfate
  8. customEvaporated