HRID29735

反应详情

EQUATION

反应方程式

HRID 29735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-2 °C

PROCEDURE

实验过程

First, 23.07 g (0.039 M) of 9-decenoxybenzyltriphenylphosphonium bromide (compound (26)) prepared in Synthetic example 1-4 and 5.91 g of terephthalaldehyde (compound (12)) were dissolved in 315 mL of ethanol. The resulting solution was cooled to −2° C., and then 25.64 g of a sodium ethoxide ethanol solution (21 percent by weight, aldrich) was added dropwise at 0° C. or less. Aging was performed at a mixture temperature of 0° C. or less for 1.5 hours and then at a mixture temperature of 10° C. to 15° C. for 2 hours. After aging, 39 g of deionized water was added dropwise. Then, the precipitated crystals were filtrated and washed with 50 mL of 60% aqueous ethanol and 30 mL of ethanol, followed by drying. Thereby, 7.12 g of 9-decenoxystilbene aldehyde (compound (27)) was produced (yield: 50.0%).

WORKUP

后处理

  1. waitat a mixture temperature of 10° C. to 15° C. for 2 hours
  2. filtrationThen, the precipitated crystals were filtrated
  3. washwashed with 50 mL of 60% aqueous ethanol and 30 mL of ethanol
  4. customby drying