HRID9673

反应详情

EQUATION

反应方程式

HRID 9673 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

A mixture of triisopropyl[(3-methylthien-2-yl)methoxy]silane (intermediate 115, 1.42 g) in tetrahydrofuran (20 ml), stirred at −78° C. under nitrogen, was treated with 1.6M butyllithium in hexanes (3.9 ml). The reaction temperature was slowly allowed to rise to 0° C. over 2 hours and then re-cooled to −78° C. 2-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.28 ml) was added and the reaction stirred at this temperature for 4 hours and then warmed to 0° C. The reaction was added to a mixture of saturated ammonium chloride and ice. The aqueous mixture was extracted with diethyl ether and the organic solution dried with brine and over sodium sulfate. Evaporation of the solvent afforded the title compound as a white solid

WORKUP

后处理

  1. temperaturere-cooled to −78° C
  2. stirringthe reaction stirred at this temperature for 4 hours
  3. temperaturewarmed to 0° C
  4. extractionThe aqueous mixture was extracted with diethyl ether
  5. dry with materialthe organic solution dried with brine and over sodium sulfate
  6. customEvaporation of the solvent