CN106478470A - The synthesis of P-aminobenzene-sulfonamide - Google Patents
The synthesis of P-aminobenzene-sulfonamide Download PDFInfo
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- CN106478470A CN106478470A CN201510535704.3A CN201510535704A CN106478470A CN 106478470 A CN106478470 A CN 106478470A CN 201510535704 A CN201510535704 A CN 201510535704A CN 106478470 A CN106478470 A CN 106478470A
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Abstract
The building-up process of P-aminobenzene-sulfonamide, including：Add 58 grams of acetanilide in the conical flask of 100mL, cool down after heating, be rapidly added 10 12 milliliters of chlorosulfonic acids, in ice-water bath, reaction is warming up to 30 40 degree and reacts 10 20 minutes after 12 hours, then reactant liquor is added in frozen water, stirring, a large amount of white solids occur, filters.White solid is added in round-bottomed flask, adds 15 20mL strong aqua ammonia, stir 100 120 minutes, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon and boil 10min, filter, be subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide.
Description
Technical field
The present invention relates to the synthesis of P-aminobenzene-sulfonamide, belong to synthesis chemical field.
Background technology
P-aminobenzene-sulfonamide, white particle or powder crystal.Odorless.Mildly bitter flavor.164.5～166.5 DEG C of fusing point.It is slightly soluble in cold water, ethanol, methanol, acetone, is soluble in boiling water, glycerol, hydrochloric acid, potassium hydroxide and sodium hydroxide solution, insoluble in benzene, chloroform, ether and petroleum ether.Use medicine pharmaceutically can be done, have inhibitory action to the growing multiplication of antibacterial.
P-aminobenzene-sulfonamide is the intermediate of herbicide sulphur grass spirit, is also the intermediate of medical sulfanilamide.Purposes is widely.
Content of the invention
The present invention provides the building-up process of P-aminobenzene-sulfonamide, including：Add 5-8 gram of acetanilide in the conical flask of 100mL, cool down after heating, be rapidly added 10-12 milliliter chlorosulfonic acid, it is warming up to 30-40 degree reaction 10-20 minute after reaction 1-2 hour in ice-water bath, then reactant liquor is added in frozen water, stirring, a large amount of white solids occur, filters.White solid is added in round-bottomed flask, adds 15-20mL strong aqua ammonia, stir 100-120 minute, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon and boil 10min, filter, be subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide.
The synthesis of P-aminobenzene-sulfonamide, the concentration of sodium bicarbonate solution is 1mol/L.
The invention has the beneficial effects as follows：The P-aminobenzene-sulfonamide of present invention preparation, preparation process is simply it is easy to operate.
Specific embodiment
Hereinafter the principle and feature of the present invention is described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1
Add 5 grams of acetanilide in the conical flask of 100mL, cool down after heating, be rapidly added 10 milliliters of chlorosulfonic acids, reaction in ice-water bath is warming up to 30 degree and reacts 10 minutes after 1 hour, then reactant liquor is added in frozen water, stirring, a large amount of white solids, filter.White solid is added in round-bottomed flask, adds 15mL strong aqua ammonia, stir 100 minutes, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon and boil 10min, filter, be subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide 10g.
Embodiment 2
Add 8 grams of acetanilide in the conical flask of 100mL, cool down after heating, be rapidly added 12 milliliters of chlorosulfonic acids, reaction in ice-water bath is warming up to 40 degree and reacts 20 minutes after 2 hours, then reactant liquor is added in frozen water, stirring, a large amount of white solids, filter.White solid is added in round-bottomed flask, adds 20mL strong aqua ammonia, stir 120 minutes, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon and boil 10min, filter, be subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide 16g.
Embodiment 3
Add 6 grams of acetanilide in the conical flask of 100mL, cool down after heating, be rapidly added 10 milliliters of chlorosulfonic acids, reaction in ice-water bath is warming up to 40 degree and reacts 20 minutes after 2 hours, then reactant liquor is added in frozen water, stirring, a large amount of white solids, filter.White solid is added in round-bottomed flask, adds 20mL strong aqua ammonia, stir 120 minutes, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon and boil 10min, filter, be subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (2)
1. the building-up process of P-aminobenzene-sulfonamide, including：5-8 gram of acetanilide is added in the conical flask of 100mL, cool down after heating, it is rapidly added 10-12 milliliter chlorosulfonic acid, it is warming up to 30-40 degree reaction 10-20 minute after reaction 1-2 hour in ice-water bath, then reactant liquor is added in frozen water, stirring, a large amount of white solids occur, filter, white solid is added in round-bottomed flask, add 15-20mL strong aqua ammonia, stirring 100-120 minute, it is subsequently adding 3mL concentrated sulphuric acid, reaction backflow 1 hour, plus activated carbon boils 10min, filter, it is subsequently adding sodium bicarbonate and be neutralized to neutrality, the white crystal being filtrated to get is exactly P-aminobenzene-sulfonamide.
2. the synthesis of P-aminobenzene-sulfonamide described in claim 1, the concentration of sodium bicarbonate solution is 1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510535704.3A CN106478470A (en) | 2015-08-28 | 2015-08-28 | The synthesis of P-aminobenzene-sulfonamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510535704.3A CN106478470A (en) | 2015-08-28 | 2015-08-28 | The synthesis of P-aminobenzene-sulfonamide |
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| Publication Number | Publication Date |
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| CN106478470A true CN106478470A (en) | 2017-03-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510535704.3A Pending CN106478470A (en) | 2015-08-28 | 2015-08-28 | The synthesis of P-aminobenzene-sulfonamide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266342A (en) * | 2017-08-04 | 2017-10-20 | 吴赣药业（苏州）有限公司 | A kind of industrial sulfanilamide (SN) production system |
-
2015
- 2015-08-28 CN CN201510535704.3A patent/CN106478470A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266342A (en) * | 2017-08-04 | 2017-10-20 | 吴赣药业（苏州）有限公司 | A kind of industrial sulfanilamide (SN) production system |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170308 |