تفاعل #217565

ord-a97517601eb0482d87c0f270b535763c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
65°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe solvent was concentrated in vacuum
  2. 2
    غسيلthe residue washed with water
  3. 3
    أخرىThe product was isolated by filtration
  4. 4
    أخرىdried in a vacuum
  5. 5
    أخرىA sample recrystallized from methanol
  6. 6
    أخرىgave 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07381723B2uspto-grants-2008_06