- Synthesis method of atropine sulfate
-
The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of atropine sulfate. The preparation method comprises the following steps: firstly preparing tropine ester, then preparing atropine, salifying to prepare atropine sulfate, and finally refining to obtain the product. In the preparation process of the tropine ester, the reaction temperature is strictly controlled to be 105-111 DEG C, and the crystallization temperature is controlled to be 0-5 DEG C, so that the yield of the tropine ester is improved. In the process of preparing atropine through reduction reaction, palladium-carbon is adopted as a catalyst, and the reaction temperature is strictly controlled to be 10-15 DEG C, so that the product quality is effectively improved. Sulfuric acid is diluted by preparing a sulfuric acid ethanol solution, and the dripping speed of the sulfuric acid ethanol solution is controlled, so that the stable quality of atropine sulfate is ensured.
- -
-
-
- An anti-choline medicine preparation method of atropine sulfate
-
The invention provides a synchronizing method of atropine sulphate. The method is characterized in that hydrolyzing methyl phenoxyacetate (II) is hydrolyzed to obtain a compound (III); the compound (III) and thionyl chloride are subjected to acylation reaction to obtain a compound (IV); the compound (IV) and 8-methyl-8-azabicyclo[3.2.1]oct-3-alchol are subjected to condensation reaction to obtain a compound (V); the compound (V) and paraformaldehyde are used for producing atropine (VI) under an alkaline condition; the atropine (VI) is salified under an acidic condition to obtain the atropine sulphate (I). The preparation method is simple in technology, high in yield, high in purity, low in monomer impurity and easy for industrial production.
- -
-
-
- Preparation method for atropine sulfate
-
The invention discloses a preparation method for atropine sulfate. The preparation method comprises the following steps: 1) adding dry powder of daturae flower into hydrochloric acid with a concentration of 1 to 4% and a volume 0.5 to 1 time of the volume of the dry powder for wetting and swelling, then adding the swollen daturae flower powder into a percolating barrel, adding the hydrochloric acid with a concentration of 1 to 4%, dipping the powder for 24 h or above and carrying out percolating so as to obtain brown-yellow stiff paste; 2) dissolving brown-yellow stiff paste in acetone, adding active carbon, carrying out decoloring and filtering, adding acid drop by drop until a pH value is less than 7 and carrying out standing at room temperature so as to obtain hyoscyamine sulfate; and 3) spreading hyoscyamine sulfate on a sample disc, putting the sample disc into a baking oven, carrying out heating for racemization, then carrying out cooling to obtain a crude atropine sulfate product, adding ethanol, carrying out dissolving under stirring and then filtering, subjecting a filtrate to crystallization overnight and then successively carrying out pressure-reduced filtering and vacuum drying so as to obtain atropine sulfate. According to the invention, the daturae flower is used as a raw material; acid water is used for percolation and extraction; total alkali is obtained through chloroform extraction; sulfuric acid is added into an acetone solution for salt forming so as to obtain hyoscyamine sulfate, then heating is carried out for racemization, and ethanol recrystallization is carried out to obtain atropine sulfate; and the method is simple in process operation, small in pollution, low in cost and suitable for industrial production.
- -
-
Paragraph 0011; 0014; 0017; 0023
(2017/06/02)
-
- CRYSTALLINE ATROPINE SULFATE
-
The present invention relates to crystalline polymorph form of Atropine sulfate and process for the preparation thereof.
- -
-
-