反应 #57549
ord-396e1a9866ed4c4b8c9948fd1834b2a0
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度The mixture was refluxed overnight
- 2workup.ADDITIONthen poured onto ice water, which
- 3其他to precipitate as a white solid
- 4其他The product was isolated by vacuum filtration
- 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).