CN1054604C - Process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride - Google Patents
Process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride Download PDFInfo
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- CN1054604C CN1054604C CN 97112089 CN97112089A CN1054604C CN 1054604 C CN1054604 C CN 1054604C CN 97112089 CN97112089 CN 97112089 CN 97112089 A CN97112089 A CN 97112089A CN 1054604 C CN1054604 C CN 1054604C
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- hydrochloride
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Abstract
The present invention discloses a method for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride, which is characterized in that under the condition that the temperature of a reaction kettle is lower than 100 DEG C, ammonium chloride is added, and then, morpholine and xylene are added; the reaction kettle is slowly heated, and the temperature can reach 80 to 110 DEG C for maintaining 30 minutes; afterwards, the reaction kettle is continuously heated and the reaction is 1.5 to 3 hours when the temperature is above 120 DEG C; after the reaction is finished, the temperature is dropped, and products are morpholine hydrochloride received by precursor of monoxydine hydrochloride. The rate of morpholine to ammonium chloride to xylene is 1 to (0.66 to 0.70) to (1.3 to 1.7) as showed in a chemical equation.
Description
The present invention relates to a kind of process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride, belong to field of medicine and chemical technology.
The moroxydine hydrochloride commodity are called moroxydine, antiviral, and the clinical control that is used for influenza, measles, varicella, zoster, its precursor salify traditional preparation process method is " acid system ", chemical equation:
Morpholine hydrochloride acid morpholine
Yet, this kind method gained morpholine hydrochloride cost height, yield is low, and is of poor quality, and wherein starting material hydrochloric acid is serious to equipment corrosion, and the production cycle is long, reacts wayward.
The present invention is directed to the problems referred to above, a kind of process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride is provided, promptly replace hydrochloric acid in the traditional method with ammonium chloride.
Task of the present invention is finished as follows: be lower than under 100 ℃ of conditions the ammonium chloride input at temperature of reaction kettle, add morpholine and dimethylbenzene again, slowly heat up, make temperature rise to 80-110 ℃, kept follow-up temperature of continuing rising 30 minutes, and reaction more than 120 ℃ 1.5-3 hour, reaction is finished, cooling, and resultant is the receptible morpholine hydrochloride of moroxydine hydrochloride; Above-mentioned morpholine, ammonium chloride, dimethylbenzene amount ratio are 1: (0.66-0.70): (1.3-1.7);
Chemical equation:
Morpholine+ammonium chloride---morpholine hydrochloride+ammonia ↑; When said process after reaction finished in 1.5-3 hour more than 120 ℃, be cooled to 70-90 ℃, add water and heat up and make material dissolution, stop to stir at 90-100 ℃, static layering divides water-yielding stratum in the decolouring still, adds gac, the gac add-on is 0.025: 1 with the ratio of morpholine, make temperature 80-90 ℃ of decolouring 30 minutes, lower the temperature crystallization after filtration pressure is expected in the crystallization kettle, blowing separates in whizzer in the time of 15 ℃, and after drying gets the finished product morpholine hydrochloride.
The present invention adopts ammonium chloride to replace hydrochloric acid synthetic hydrochloric acid Wirumin precursor morpholine hydrochloride, can reduce starting material and energy cost, the yield height, and quality is good, etching apparatus not, the production cycle shortens, and reaction simultaneously is easy to control, steady quality.
Embodiment:
At temperature of reaction kettle is under 70 ℃ of conditions, after dropping into ammonium chloride 55Kg, add morpholine 88Kg and dimethylbenzene 150Kg and start stirring, open the cooling for reflux system, the material steam cooling for reflux, ammonia is discharged, and slowly heats up reaction more than 120 ℃ 3 hours, and this process morpholine hydrochloride as precursor of monoxydine hydrochloride is synthetic to finish; Obtain moroxydine hydrochloride, continue to be cooled to 80 ℃, add two cyanogen ammonium 84Kg, after slowly heat up, reaction more than 136 ℃ 3 hours, reaction is finished, and cools to 100 ℃, adds water 120Kg, intensification makes material dissolution, stop to stir at 90-100 ℃, static layering divides water-yielding stratum in the decolouring still, add gac 5Kg, make temperature dewater 30 minutes after filtration pressure is expected in the crystallization kettle cooling, crystallization at 80-90 ℃, at 15 ℃ of blowings in whizzer, obtain crude product with 0.8 times of alcohol immersion, then in whizzer, separate, the dry finished product moroxydine hydrochloride (moroxydine) that gets; When said process more than 120 ℃ the reaction 3 hours, after be cooled to 80 ℃, add entry 60Kg, intensification makes material dissolution, stops to stir static layering at 90-100 ℃, divide water-yielding stratum in decolouring in still, add gac 2.5Kg, make temperature 80-90 ℃ of decolouring 30 minutes, after filtration pressure is expected in the crystallization kettle, cooling, crystallization separates in whizzer at 15 ℃ of blowings, and after drying gets the finished product morpholine hydrochloride.
Claims (2)
1, a kind of process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride, it is characterized in that: be lower than under 100 ℃ of conditions the ammonium chloride input at temperature of reaction kettle, add morpholine and dimethylbenzene again, slowly heat up, make temperature rise to 80-110 ℃, kept 30 minutes, follow-up temperature of continuing rising, and reaction more than 120 ℃ 1.5-3 hour, reaction is finished, cooling, resultant are that the above-mentioned morpholine of morpholine hydrochloride, ammonium chloride, dimethylbenzene weight ratio are 1: (0.66-0.70): (1.3-1.7), and chemical equation:
Morpholine+hydrochloric acid---morpholine hydrochloride+ammonia ↑.
2, process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride as claimed in claim 1, it is characterized in that: when said process after reaction finished in 1.5-3 hour more than 120 ℃, be cooled to 70-90 ℃, add the water intensification and make material dissolution, stop to stir at 90-100 ℃, static layering, divide water-yielding stratum in the decolouring still, add gac, the gac add-on is 0.025: 1 with the ratio of morpholine weight, makes temperature 80-90 ℃ of decolouring 30 minutes, after expecting in the crystallization kettle, filtration pressure lowers the temperature, crystallization, blowing separates in whizzer in the time of 15 ℃, and after drying gets the finished product morpholine hydrochloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97112089 CN1054604C (en) | 1997-05-22 | 1997-05-22 | Process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97112089 CN1054604C (en) | 1997-05-22 | 1997-05-22 | Process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1171398A CN1171398A (en) | 1998-01-28 |
| CN1054604C true CN1054604C (en) | 2000-07-19 |
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ID=5172089
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97112089 Expired - Fee Related CN1054604C (en) | 1997-05-22 | 1997-05-22 | Process for preparing morpholine hydrochloride as precursor of monoxydine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054604C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311421A (en) * | 2014-09-29 | 2015-01-28 | 张家港市三联化工科技有限公司 | MAQ refining treatment method |
| CN112812041B (en) * | 2021-02-01 | 2022-12-20 | 西安石油大学 | Cyclohexylbiguanide hydrochloride and preparation method thereof |
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1997
- 1997-05-22 CN CN 97112089 patent/CN1054604C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1171398A (en) | 1998-01-28 |
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