反应 #2487445

反应方程式

7-fluoro-2,1,3-benzoselenadiazole-4-sulfonyl chloride

N,N-diethylethylenediamine

triethylamine

→

7-fluoro-N-[2-(dimethylamino)ethyl]-2,1,3-benzoselenadiazole-4-sulfonamide

收率 73.7%

溶剂

acetonitrile

反应条件

后处理

1. 1
   其他The reaction mixture was evaporated to dryness in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in CH2Cl2
3. 3
   其他chromatographed on silica gel

实验过程

7-fluoro-2,1,3-benzoselenadiazole-4-sulfonyl chloride (75 mg) was dissolved in 3 ml of acetonitrile. After the addition of N,N-diethylethylenediamine (22 mg) and triethylamine (351), the mixture was stirred on ice for 30 min. The reaction mixture was evaporated to dryness in vacuo and the residue was dissolved in CH2Cl2 and chromatographed on silica gel using CH2Cl2-CH3OH (93:7) to yield 7-fluoro-N-[2-(dimethylamino)ethyl]-2,1,3-benzoselenadiazole-4-sulfonamide (49 mg, 56%) as red powder. mp: 117-120° C. 1H-NMR δH8.09 (1H, d, J=7.5 Hz), 7.24 (1H, d, J=7.5 Hz), 2.93 (2H, t, J=6.7 Hz), 2.27 (2H, t, J=6.7 Hz), 1.98 (6H, s) in CD3OD; ESI-MSm/z 353 [(M+H)+]

来源