HRID1918324

反应详情

EQUATION

反应方程式

HRID 1918324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

50.0 g of [2-(3-bromo-phenyl)-ethoxy]-tert-butyl-dimethyl-silane were dissolved in 500 ml of anhydrous THF. 64.6 ml of a 2.7 M solution of n-butyllithium in n-heptane were added dropwise at −70° C. The mixture was stirred for 1 h at −70° C. Then 40.2 ml of triisopropyl borate were added dropwise at −70° C. Stirring was continued for 30 min at −70° C. and the mixture allowed to warm up to −20° C. 500 ml of water were added and the mixture was extracted three time with 500 ml each of DCM. The combined organic layers were dried with magnesium sulfate and evaporated to yield 43.6 g of the title compound.

WORKUP

后处理

  1. stirringStirring
  2. waitwas continued for 30 min at −70° C.
  3. temperatureto warm up to −20° C
  4. extractionthe mixture was extracted three time with 500 ml each of DCM
  5. dry with materialThe combined organic layers were dried with magnesium sulfate
  6. customevaporated