反应 #57549

ord-396e1a9866ed4c4b8c9948fd1834b2a0

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07420066B2uspto-grants-2008_09