反応 #2487444

反応方程式

N-thionylaniline

3-fluoro-O-phenylene diamine

→

4-fluoro-2,1,3-benzothiadiazole

反応条件

後処理

1. 1
   その他4-Fluoro-2,1,3-benzothiadiazole was synthesized
2. 2
   ろ過After the solvent was filtered off
3. 3
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane
4. 4
   洗浄the solution was washed with 10% HCl solution and water
5. 5
   その他The organic layer was dried
6. 6
   その他evaporated to dryness
7. 7
   その他Purification by chromatography on a silica gel column with chloroform as an eluent

実験手順

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.

出典