反应 #56594
ord-7b03299eb0ab4ce5adf307e56e52b766
反应方程式
4-hydroxy-3-methyl4′-phenylazo-azobenzene
triphenylphosphine
diethyl azodicarboxylate
4-hydroxybutylacrylate
→
4-(4-Acryloyloxybutyloxy)-3-methyl-4′-phenylazo-azobenzene
反应物
试剂
无
反应条件
温度
-30°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.ADDITIONAfter complete addition
- 2浓缩concentrated to dryness
- 3过滤The obtained yellow-red residue was purified by filtration on silica
- 4其他to give 0.65 g of pure yellow-orange crystalys
实验过程
To a solution of 0.63 g of 4-hydroxy-3-methyl4′-phenylazo-azobenzene, 1.05 g of triphenylphosphine and 0.58 g of 4-hydroxybutylacrylate in 10 ml THF; which was cooled to −30° C., was added dropwise a solution of 0.70 g of diethyl azodicarboxylate in 5 ml THF. After complete addition, the reaction mixture was stirred for further 45 min at room temperature, and then concentrated to dryness. The obtained yellow-red residue was purified by filtration on silica using methylenechloride as the eluent to give 0.65 g of pure yellow-orange crystalys; λmax. (CB 483): 395 nm.