HRID1980531

反应详情

EQUATION

反应方程式

HRID 1980531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 12.8 g (0.052 mol) of chloromethyl(diethoxy)phenylsilane, 9.4 g (0.062 mol) of sodium iodide and 0.21 g (0.52 mol) of tricaprylylmethylammonium chloride (Aliquat®336) in 10 of ethyl alcohol was refluxed for 12 hours, cooled, filtered, and evaporated. The filtrate was diluted with water and extracted with ether. The ether solution was washed with brine, dried over magnesium sulfate, evaporated, and distilled to provide 8.7 g (50%) of the title compound as a clear liquid: b.p. 86°-100° (0.15 mm); nD19 1.5204; ir (neat) 2980, 1590, 1480, 1430, 1390, 1290, 1165 cm-1 ; nmr (CDCl3) 1.25 (6H, t, J=7), 2.15 (2H, s), 3.85 (3H, q, J=7) and 7.3-7.9 (5H, m).

WORKUP

后处理

  1. temperaturewas refluxed for 12 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. customevaporated
  5. additionThe filtrate was diluted with water
  6. extractionextracted with ether
  7. washThe ether solution was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. customevaporated
  10. distillationdistilled