تفاعل #46458

ord-c9bb23be4d014b61b2df65620189bc16

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe DMF was removed under vacuum, and 1M HCl
  2. 2
    workup.ADDITIONwas added until the residue
  3. 3
    استخلاصThe mixture was extracted with ethyl acetate
  4. 4
    تجفيفthe combined organic phase was dried over magnesium sulfate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

2-Bromo-4-methyl-6-iodophenol (7.82 gm, 25 mmol) and cinnamyl bromide (4.93 g, 25 mmol) were added to DMF (20 ml). Diisopropylethylamine (5.3 ml, 30.4 mmol) was added and the mixture heated to 60° C. for 15 minutes and then allowed stir for 16 hours at room temperature. The DMF was removed under vacuum, and 1M HCl was added until the residue was acidic. The mixture was extracted with ethyl acetate, and the combined organic phase was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give 1-bromo-3-iodo-5-methyl-2-(3-phenylallyloxy)-benzene (10.86 g, 100% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741326B2uspto-grants-2010_06