반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].[S].[CH2:11](N)[CH2:12][NH2:13]>>[Br:1][C:2]1[CH:3]=[C:4]([C:5]2[NH:13][CH2:12][CH2:11][N:6]=2)[CH:7]=[CH:8][CH:9]=1참가 물질
4
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).
후처리
- temperatureThe mixture was refluxed overnight
- additionthen poured onto ice water, which
- customto precipitate as a white solid
- customThe product was isolated by vacuum filtration
- customdried in a vacuum oven (545 mg, 88%)
출처 및 근거
- ORD 기록
- ord-396e1a9866ed4c4b8c9948fd1834b2a0
- 출처 데이터셋
- uspto-grants-2008_09
- 특허 번호
- US07420066B2
연결된 노트
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