تفاعل #57549

ord-396e1a9866ed4c4b8c9948fd1834b2a0

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was refluxed overnight
  2. 2
    workup.ADDITIONthen poured onto ice water, which
  3. 3
    أخرىto precipitate as a white solid
  4. 4
    أخرىThe product was isolated by vacuum filtration
  5. 5
    أخرىdried in a vacuum oven (545 mg, 88%)

الإجراء التجريبي

To a solution of 3-bromobenzonitrile (500 mg, 2.75 mmol) in ethylenediamine (3.5 mL) was added sulfur (44 mg, 1.4 mmol). The mixture was refluxed overnight then poured onto ice water, which caused the product to precipitate as a white solid. The product was isolated by vacuum filtration and dried in a vacuum oven (545 mg, 88%). 1H-NMR (CDCl3) δ 7.93 (t, J=1.7 Hz, 1H), 7.68 (ddd, J=7.8, 1.2, 1.2 Hz, 1H), 7.56 (dddd, J=7.8, 0.9, 0.9, 0.9 Hz, 1H), 7.26 (dd, J=10.5, 8.0 Hz, 1H), 3.78 (br s, 4H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07420066B2uspto-grants-2008_09