反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitat a mixture temperature of 10° C. to 15° C. for 2 hours
- filtrationThen, the precipitated crystals were filtrated
- washwashed with 50 mL of 60% aqueous ethanol and 30 mL of ethanol
- customby drying