تفاعل #462200

ord-10ae76f6ec0f4443944228377f5b406d

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) δ1.15-1.26 (dt, 9), 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: US05484556uspto-grants-1996_01