تفاعل #59492

ord-7f9a6aad03f3423b9c5a65a32fd0e897

المذيبات

ظروف التفاعل

درجة الحرارة
22°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe mixture was filtered
  2. 2
    أخرىevaporated to dryness under reduced pressure
  3. 3
    أخرىThe residue was triturated with the mixture of ether (8.2 ml) and water (1.4 ml) at the ice bath temperature
  4. 4
    ترشيحThe product was collected by filtration
  5. 5
    غسيلwashed with cold ether
  6. 6
    أخرىdried under reduced pressure

الإجراء التجريبي

A mixture of 2,5-bis(benzyloxy)phenol (0.28 g), 2-bromoacetophenone (0.22 g), potassium hydrogen-carbonate (0.25 g) and 18-Crown-6 (3 mg) in acetonitrile (4.2 ml) was stirred at 22° C. for one week. The mixture was filtered and evaporated to dryness under reduced pressure. The residue was triturated with the mixture of ether (8.2 ml) and water (1.4 ml) at the ice bath temperature. The product was collected by filtration, washed with cold ether and dried under reduced pressure. Yield is 0.14 g. 1H NMR (DMSO-d6) δ=4.98 (s, 2H), 5.06 (s, 2H), 5.58 (s, 2H), 6.51 (dd, J=8.9, 2.3 Hz, 1H), 6.68 (d, J=2.3 Hz, 1H), 6.94 (d, J=8.9 Hz, 1H), 7.28-8.03 (m, 15H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425568B2uspto-grants-2008_09