反应 #2487444
ord-a8158a7d3c5d48899f27b304a56fbc76
反应方程式
N-thionylaniline
3-fluoro-O-phenylene diamine
→
4-fluoro-2,1,3-benzothiadiazole
反应条件
温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他4-Fluoro-2,1,3-benzothiadiazole was synthesized
- 2过滤After the solvent was filtered off
- 3workup.DISSOLUTIONthe residue was dissolved in dichloromethane
- 4洗涤the solution was washed with 10% HCl solution and water
- 5其他The organic layer was dried
- 6其他evaporated to dryness
- 7其他Purification by chromatography on a silica gel column with chloroform as an eluent
实验过程
4-Fluoro-2,1,3-benzothiadiazole was synthesized according to the method in which N-thionylaniline (0.49 g, 3.5 mmol) was added to a solution of the 3-fluoro-O-phenylene diamine (200 mg, 1.6 mmol) in foluen (2 ml) The reaction mixture was heated at 100-120° C. for 4 hr. After the solvent was filtered off, the residue was dissolved in dichloromethane and the solution was washed with 10% HCl solution and water, successively. The organic layer was dried and evaporated to dryness. Purification by chromatography on a silica gel column with chloroform as an eluent gave 4-fluoro-2,1,3-benzothiadiazole as pal yellow oil. Confirmed data of the obtained chemical compound is shown as follows.