تفاعل #56594
ord-7b03299eb0ab4ce5adf307e56e52b766
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
-30°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONAfter complete addition
- 2تركيزconcentrated to dryness
- 3ترشيحThe obtained yellow-red residue was purified by filtration on silica
- 4أخرىto give 0.65 g of pure yellow-orange crystalys
الإجراء التجريبي
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.