HRID1348534

反应详情

EQUATION

反应方程式

HRID 1348534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

150 ml of a 2.3 M sodium cyclopentadienide solution in tetrahydrofurane (346 mmol) is slowly added to a solution of 68.2 g (346 mmol) 2-trimethylsiloxy-1-bromo-ethane in tetrahydrofurane. The immediate formation of a pinkish solid is observed. The reaction is maintained under stirring for 12 hours. Then, an ammonium chloride aqueous solution is added. The organic phase is extracted, dried with magnesium sulphate and the volatile part is distilled under vacuum, obtaining an orange oil. This oil is distilled in order to obtain a colourless oil. (Tb.: 63–65° C., 0.02 bar (15 mmHg.)). (40.3 g, 221 mmol. Yield:64%). 1H-NMR (CDCl3): 6.50–6.00 (m,3H), 3.75 (m, 2H), 2.95 (m, 2H), 2.65 (m, 2H), 0.15 (s, 9H).

WORKUP

后处理

  1. temperatureThe reaction is maintained
  2. extractionThe organic phase is extracted
  3. dry with materialdried with magnesium sulphate
  4. distillationthe volatile part is distilled under vacuum
  5. customobtaining an orange oil
  6. distillationThis oil is distilled in order
  7. customto obtain a colourless oil
  8. custom(Tb.: 63–65° C., 0.02 bar (15 mmHg.))