تفاعل #640556

ord-fa8f6dad7ad047a4b8e62d003cb4b1e2

معادلة التفاعل

O=C(C(=O)c1ccc(Br)cc1)c1ccc(Br)cc1
4,4′-dibromobenzil
Nc1ccccc1N
o-phenylenediamine
Brc1ccc(-c2nc3ccccc3nc2-c2ccc(Br)cc2)cc1
2,3-bis(4-bromophenyl)quinoxaline
المردود 92.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلThe reaction solution was washed with water
  2. 2
    درجة الحرارةafter being cooled to room temperature
  3. 3
    استخلاصAn aqueous layer was extracted with chloroform
  4. 4
    غسيلwashed with a saturated saline solution
  5. 5
    تجفيفThe organic layer was dried over magnesium sulfate
  6. 6
    ترشيحfiltered
  7. 7
    أخرىcondensed

الإجراء التجريبي

A chloroform solution (200 mL) of 30.0 g (81.5 mmol) of 4,4′-dibromobenzil and 9.00 g (83.2 mmol) of o-phenylenediamine was heated and refluxed at 80° C. for 3 hours under nitrogen atmosphere. The reaction solution was washed with water after being cooled to room temperature. An aqueous layer was extracted with chloroform. This extracted aqueous layer and an organic layer were put together and washed with a saturated saline solution. The organic layer was dried over magnesium sulfate and filtered. The filtrate was condensed to obtain 33 g (yield: 92%) of objective 2,3-bis(4-bromophenyl)quinoxaline as a white solid. Synthetic scheme of Step 1 is shown in the following (d-1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08048540B2uspto-grants-2011_11