반응 #57549

ord-396e1a9866ed4c4b8c9948fd1834b2a0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07420066B2uspto-grants-2008_09