تفاعل #56734
ord-3f44aa63a8b8417582fb109a69f778d9
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
65°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزThe solvent was concentrated in vacuum
- 2غسيلthe residue washed with water
- 3أخرىThe product was isolated by filtration
- 4أخرىdried in a vacuum
- 5أخرىA sample recrystallized from methanol
- 6أخرىgave m.p. 93-94° C.
الإجراء التجريبي
97.5 g (0.51 mole) of the sodium salt of 5-nitroguaiacol was dissolved in one liter of DMF and 1.5 equivalents of allyl bromide added. The reaction was heated to 65° C. for two hours, after which time much of the dark color had discharged and tlc (1:1 CH2Cl2/hexane) indicated loss of starting material. The solvent was concentrated in vacuum and the residue washed with water. The product was isolated by filtration and dried in a vacuum. This gave 112 g of pale yellow solid. A sample recrystallized from methanol, gave m.p. 93-94° C.