HRID1198561

反应详情

EQUATION

反应方程式

HRID 1198561 的结构方程式

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

To a stirred solution of the protected nitrophenol (3.05 g, 10 mmol) (Example 34a part i) in dry THF (100 ml) at -40° C. under nitrogen was added 1M vinyl magnesium bromide in the THF (35 ml) over 5 minutes. After stirring for a further three quarters of an hour at -40° C., the reaction mixture was poured into aqueous ammonium chloride and extracted into diethyl ether. The combined organic extracts were dried, filtered and evaporated in vacuo. The product was purified by column chromatography on silica, eluting with 12.5% ethyl acetate in hexane, to give a pale yellow solid.

WORKUP

后处理

  1. extractionextracted into diethyl ether
  2. customThe combined organic extracts were dried
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe product was purified by column chromatography on silica
  6. washeluting with 12.5% ethyl acetate in hexane
  7. customto give a pale yellow solid