A kind of synthetic method of 2-chloro-6-bromoaniline
A synthesis method, bromoaniline technology, applied in the field of synthesis of 2-chloro-6-bromoaniline, can solve the problems of emission pollution, utilization rate of halogen atoms is only 50%, dangerous operation, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0029] The first step, the synthesis of compound 2
[0030] Under anhydrous and oxygen-free conditions, 1 mmol of sulfanilamide was dissolved in 8 mL of ethanol, and then 1 mmol of NCS powder was added, and reacted at 30° C. for 19 h. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the organic layer was washed with 5 mL of saturated potassium carbonate solution and 5 mL of saturated brine. The organic layer was dried over anhydrous sodium sulfate, and column chromatography (dichloromethane: ethyl acetate 7:1) gave 188 mg of light yellow powder with a yield of 90%.
[0031] The second step, the synthesis of compound 3
[0032] Under anhydrous and oxygen-free conditions, 207mg 3-chloro-p-aminobenzenesulfonamide (1mmol), 178mg NBS powder (1mmol) and solvent DMF 8mL were added to a 100mL two-necked flask, and reacted at 30°C for 5 hours. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the organic layer was washed with...
Embodiment 2
[0036] The first step, the synthesis of compound 2
[0037] Under anhydrous and oxygen-free conditions, 1 mmol of p-aminobenzenesulfonamide was dissolved in 8 mL of acetonitrile, and then 1.2 mmol of NCS powder was added, and reacted at 20° C. for 19 h. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the organic layer was washed with 5 mL of saturated potassium carbonate solution and 5 mL of saturated brine. The organic layer was dried over anhydrous sodium sulfate, and column chromatography (dichloromethane: ethyl acetate 7:1) gave 188 mg of light yellow powder with a yield of 90%.
[0038] The second step, the synthesis of compound 3
[0039] Under anhydrous and oxygen-free conditions, 207mg 3-chloro-p-aminobenzenesulfonamide (1mmol), 214mg NBS powder (1.2mmol) and solvent acetone 8mL were added to a 100mL two-necked flask, and reacted at 20°C for 6 hours. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the orga...
Embodiment 3
[0043] The first step, the synthesis of compound 2
[0044]Under anhydrous and oxygen-free conditions, 1 mmol of p-aminobenzenesulfonamide was dissolved in 4 mL of methanol, and then 1 mmol of NCS powder was added, and reacted at 20°C for 10 h. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the organic layer was washed with 5 mL of saturated potassium carbonate solution and 5 mL of saturated brine. The organic layer was dried over anhydrous sodium sulfate, and column chromatography (dichloromethane: ethyl acetate 7:1) gave 188 mg of light yellow powder with a yield of 85%.
[0045] The second step, the synthesis of compound 3
[0046] Under anhydrous and oxygen-free conditions, 207mg 3-chloro-p-aminobenzenesulfonamide (1mmol), 178mg NBS powder (1mmol) and solvent acetonitrile 8mL were added to a 100mL two-necked flask, and reacted at 20°C for 3 hours. The solvent was evaporated, the residue was extracted with 30 mL of ether, and the organic la...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More