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
- 50 °C
PROCEDURE
实验过程
In a 2-liter three-necked flask equipped with a stirring device and a nitrogen substituting device, 169.6 g of 1,3-diphenyl-2-n-hexyl-2-propen-1-ol, 0.4 milliliters of trifluoroacetic acid and 17 g of a Pd-C catalyst (a 5% product, containing 55.9% of water) were introduced, and stirred at 50° C. and contacted with hydrogen gas. After stirring for 30 hours, the catalyst was filtered off, water was added, and an extraction was carried out with n-heptane. After washing with sodium hydrogencarbonate and water, the solution was dried with anhydrous sodium sulfate. After removing off the solvent by a rotary evaporator and dissolving the residue in a small amount of n-heptane, a separating operation was carried out by a column chromatography with silica gel. By removing off the solvent again and carrying out a distillation under a decreased pressure, to obtain 98.9 g of 1,3-diphenyl-2-n-hexyl propane as colorless liquid.
WORKUP
后处理
- customIn a 2-liter three-necked flask equipped with a stirring device
- additionwere introduced
- stirringAfter stirring for 30 hours
- filtrationthe catalyst was filtered off
- additionwater was added
- extractionan extraction
- washAfter washing with sodium hydrogencarbonate and water
- dry with materialthe solution was dried with anhydrous sodium sulfate
- customAfter removing off the solvent
- customby a rotary evaporator
- dissolutiondissolving the residue in a small amount of n-heptane
- customBy removing off the solvent again
- distillationa distillation under a decreased pressure