تفاعل #353180

ord-28f4243e5bd54a48a1f385510c453ce2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىhad crystallized out of solution
  2. 2
    ترشيحThe crystals were filtered
  3. 3
    غسيلwashed with toluene (3×50 mL) and pentane (3×50 mL)
  4. 4
    أخرىdried

الإجراء التجريبي

To a mixture of α,α'-dichloro-o-xylene (15.0 g, 86.0 mmol) in toluene (200 ml) was added triethylphosphine (6.3 ml, 43.0 mmol) under argon gas. The reaction mixture was stirred for several days at room temperature under argon after which time the triethylphosphonium chloride salt had crystallized out of solution. The crystals were filtered and washed with toluene (3×50 mL) and pentane (3×50 mL) and dried: 1H NMR (CDCl3) δ 1.15-1.26 (dt, 9H), 2.58-2.69 (m, 6H), 4.39-4.44 (d, 2H), 4.87 (s, 2H), 7.31-7.34 (dd, 2H), 7.43-7.46 (dd, 1H), 7.50-7.54 (m, 1H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05650099uspto-grants-1997_07