CN117024251A - Method for preparing medicinal grade 1, 3-butanediol - Google Patents
Method for preparing medicinal grade 1, 3-butanediol Download PDFInfo
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- CN117024251A CN117024251A CN202311015928.2A CN202311015928A CN117024251A CN 117024251 A CN117024251 A CN 117024251A CN 202311015928 A CN202311015928 A CN 202311015928A CN 117024251 A CN117024251 A CN 117024251A
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- butanediol
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- preparing pharmaceutical
- pharmaceutical grade
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 235000019437 butane-1,3-diol Nutrition 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 230000001954 sterilising effect Effects 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims description 34
- 239000012279 sodium borohydride Substances 0.000 claims description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 abstract description 30
- 239000002253 acid Substances 0.000 abstract description 2
- 150000001299 aldehydes Chemical class 0.000 abstract 1
- 239000000047 product Substances 0.000 description 23
- 238000007670 refining Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004659 sterilization and disinfection Methods 0.000 description 6
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- 238000010668 complexation reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- 241000219000 Populus Species 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000546 pharmaceutical excipient Substances 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application provides a method for preparing medicinal-grade 1, 3-butanediol, and relates to the field of pharmacy. The method for preparing the medical grade 1, 3-butanediol comprises the following steps: mixing industrial-grade 1, 3-butanediol with a reducing agent, stirring for reaction, and performing solid-liquid separation to obtain a reaction solution; mixing the reaction liquid with a stable complexing agent, heating, distilling under reduced pressure, sterilizing, and filtering to obtain the medicinal 1, 3-butanediol. The method for preparing the medical grade 1, 3-butanediol can refine the impurity aldehydes and acid impurities in the crude 1, 3-butanediol to almost undetected, effectively improves the product purity, meets the medical requirements, and solves the problem of overproof commercial industrial grade 1, 3-butanediol impurities.
Description
Technical Field
The application relates to the technical field of pharmacy, in particular to a method for preparing medicinal grade 1, 3-butanediol.
Background
1, 3-butanediol is an important raw material for alkyd resins and polyester resins, and the excellent product characteristics of the raw material can be applied to a plurality of downstream application fields. The 1, 3-butanediol can be applied to the industries of resin, chemical industry, food, medicine and the like, the monocarboxylic monoester of the 1, 3-butanediol is an excellent plasticizer for PVC and other plastics, and can be prepared into unsaturated polyester resin together with monomers such as phthalic anhydride, maleic anhydride and the like.
The existing industrialized production processes include an acetaldehyde condensation hydrogenation process and a condensation hydrolysis reaction of propylene and formaldehyde. According to the comparison of different processes, the acetaldehyde condensation hydrogenation process is a mainstream process for producing 1, 3-butanediol, has high conversion rate, good selectivity and biological activity, and the purity of the product 1, 3-butanediol is higher, so that the problem that residual aldehyde impurities can be inevitably generated in industrial-grade 1, 3-butanediol is seen.
1, 3-butanediol is used as a pharmaceutical adjuvant and is mainly received in United states and Indian pharmacopoeia. Wherein the United states pharmacopoeia requirements are set forth in Table 1.
Table 1: U.S. pharmacopoeia 1, 3-butanediol quality standard
Therefore, 1, 3-butanediol is taken as a pharmaceutic adjuvant, related substances must meet specific requirements, any single impurity must be less than or equal to 0.1%, and commercial industrial grade and cosmetic grade 1, 3-butanediol are difficult to meet the requirements of pharmaceutical grade.
Therefore, development of an effective 1, 3-butanediol refining and purifying process is urgently needed at present to obtain a medicinal grade 1, 3-butanediol product with low impurity content, high product purity and medicinal requirements.
Disclosure of Invention
The present application aims to provide a method for preparing pharmaceutical grade 1, 3-butanediol, which solves the above problems.
In order to achieve the above purpose, the application adopts the following technical scheme:
a process for preparing pharmaceutical grade 1, 3-butanediol comprising:
mixing industrial-grade 1, 3-butanediol with a reducing agent, stirring for reaction, and performing solid-liquid separation to obtain a reaction solution;
mixing the reaction liquid with a stable complexing agent, heating, distilling under reduced pressure, sterilizing, and filtering to obtain the medicinal 1, 3-butanediol.
Preferably, the temperature of the stirring reaction is between-10 and 50 ℃ for 0.5 to 4 hours.
Preferably, the temperature of the stirring reaction is 0 to 5 ℃ for 1-2h.
Alternatively, the temperature of the stirring reaction may be any value of-10 ℃, -5 ℃, 0 ℃, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃ or-10 to 50 ℃ and the time may be any value of 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h or 0.5 to 4h.
Preferably, the reducing agent comprises sodium borohydride.
Preferably, the sodium borohydride is used in an amount of 0.01% -0.5% of the mass of the technical grade 1, 3-butanediol.
Preferably, the sodium borohydride is used in an amount of 0.1% by mass of the technical grade 1, 3-butanediol.
Alternatively, the sodium borohydride may be used in an amount of any of 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, or between 0.01% and 0.5% by mass of the technical grade 1, 3-butanediol.
Preferably, the stabilizing complexing agent comprises stannous oxide.
Preferably, the stannous oxide is used in an amount of 0.05% -0.5% by mass of the technical grade 1, 3-butanediol.
Preferably, the stannous oxide is used in an amount of 0.1% by mass of the technical grade 1, 3-butanediol.
Alternatively, the stannous oxide may be used in an amount of any one of 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5% or between 0.05% and 0.5% by mass of the technical grade 1, 3-butanediol.
Preferably, the temperature of the reduced pressure distillation is 100-120 ℃ and the vacuum degree is not higher than 5kPa.
Alternatively, the temperature of the reduced pressure distillation may be 100 ℃,110 ℃,120 ℃ or any value between 100 and 120 ℃, and the vacuum degree is preferably not higher than 1kPa.
Compared with the prior art, the application has the beneficial effects that:
according to the method for preparing the medical grade 1, 3-butanediol, the reducer is added into the industrial grade 1, 3-butanediol crude product, the reaction is fully stirred and carried out, and the reaction liquid is obtained by filtration; and adding a stable complexing agent into the reaction solution, and then carrying out reduced pressure distillation to obtain the medical grade 1, 3-butanediol. The method can refine the impurity aldehydes and acid impurities in the 1, 3-butanediol crude product to almost undetected, effectively improves the product purity, meets the medicinal requirement, and solves the problem of overproof commercial industrial grade 1, 3-butanediol impurities.
Detailed Description
Embodiments of the present application will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The raw material information and sources used in the following specific examples are shown in Table 2:
table 2 raw material description
| Sequence number | Raw materials | Purity/information | Source |
| 1 | 1, 3-butanediol | Industrial grade | Japanese cellophane chemical industry Co Ltd |
| 2 | Sodium borohydride | Reagent grade | Poplar chemical Co., ltd |
| 3 | Activated carbon | Pharmaceutical grade | SHANGHAI JINHU ACTIVATED CARBON Co.,Ltd. |
| 4 | Stannous oxide | Industrial grade | Poplar chemical Co., ltd |
Example 1
The embodiment provides a method for preparing medical grade 1, 3-butanediol, which specifically comprises the following steps:
100g of crude 1, 3-butanediol (purity is 99.67%, and maximum single impurity is 0.17%) is added into a three-neck flask, a thermometer, a condenser tube and the like are arranged, the temperature is controlled to be 0-5 ℃, 0.1g of sodium borohydride is slowly added, the temperature is kept and stirred for 0.5h, filtration is carried out, stannous oxide 0.1g is added into refined solution, the temperature is controlled to be 110+/-3 ℃, the pressure is controlled to be less than or equal to 3kPa for reduced pressure concentration, about 5g of front cut is trapped and concentrated until about 5g of concentrated mother solution remains, the reduced pressure concentration is stopped, the temperature is reduced to room temperature, the refined pharmaceutical grade 1, 3-butanediol 88.4g is obtained through sterilization and filtration, and the color of the refined product is colorless. The purity of the product is 99.91 percent, the maximum single impurity is 0.03 percent, and the product meets the quality requirement of USP43-NF 38.
Example 2
The embodiment provides a method for preparing medical grade 1, 3-butanediol, which specifically comprises the following steps:
100g of crude 1, 3-butanediol (purity is 99.73 percent and maximum single impurity is 0.15 percent) is added into a three-neck flask, a thermometer, a condenser pipe and the like are arranged, the temperature is controlled to be 10-15 ℃, 0.2g of sodium borohydride is slowly added, the temperature is kept and stirred for 0.5h, the filtration is carried out, 0.1g of stannous oxide is added into the refined solution, the temperature is controlled to be 105+/-3 ℃, the pressure is controlled to be less than or equal to 1kPa for reduced pressure concentration, about 3g of front cut is trapped and concentrated until about 3g of concentrated mother solution remains, the reduced pressure concentration is stopped, the temperature is reduced to room temperature, 92.4g of refined pharmaceutical grade 1, 3-butanediol is obtained through sterilization and filtration, and the color of the refined product is colorless. The purity of the product is 99.79%, the maximum single impurity is 0.07%, and the product meets the quality requirement of USP43-NF 38.
Example 3
The embodiment provides a method for preparing medical grade 1, 3-butanediol, which specifically comprises the following steps:
100g of crude 1, 3-butanediol (purity is 99.45%, single impurity is 0.204% at maximum) is added into a three-neck flask, a thermometer, a condenser tube and the like are arranged, the temperature is controlled to 45 ℃, 0.05g of sodium borohydride is slowly added, the temperature is kept for 2.0h, the mixture is filtered, 0.2g of stannous oxide is added into the refined solution, the temperature is controlled to 115+/-3 ℃, the pressure is controlled to be less than or equal to 5kPa for reduced pressure concentration, about 3g of front cut is trapped and concentrated until about 3g of concentrated mother solution is left, the reduced pressure concentration is stopped, the temperature is reduced to room temperature, 90.6g of refined pharmaceutical grade 1, 3-butanediol is obtained through sterilization and filtration, and the color of the refined product is colorless. The purity of the product is 99.85%, the maximum single impurity is 0.06%, and the product meets the quality requirement of USP43-NF 38.
In summary, the purity of the refined products obtained in examples 1-3 is obviously and effectively improved, the maximum single impurity is reduced, the color of the product becomes light, and the obtained product meets the high-purity pharmaceutical grade 1, 3-butanediol of pharmaceutical requirements.
Further, in order to determine the optimal temperature for distillation refining of the stannous oxide complex impurities in the second step, the experimental scheme is designed as follows (examples 4-8) except that the distillation temperature is changed, and the other components and the process conditions are unchanged:
the feeding ratio is as follows: 100g of technical grade 1, 3-butanediol; 0.2g of sodium borohydride; 0.1g of stannous oxide.
Distillation temperature (100 ℃,110 ℃,120 ℃,130 ℃,140 ℃).
The detailed operation steps are as follows:
adding 100g of crude 1, 3-butanediol (purity 99.43%, maximum single impurity 0.23%) into a three-neck flask, placing a thermometer, a condenser tube and the like, controlling the temperature to 10-15 ℃, slowly adding 0.2g of sodium borohydride, keeping the temperature, stirring for 0.5h, filtering, adding 0.1g of stannous oxide into the refined solution, concentrating under reduced pressure at the temperature of 100 ℃;110 ℃;120 ℃ and 130 ℃ and 140 ℃ under the control pressure of about 1kPa, intercepting about 3g of the front cut fraction, concentrating until about 5g of concentrated mother liquor remains, stopping concentrating under reduced pressure, cooling to room temperature, sterilizing and filtering to obtain refined 1, 3-butanediol, calculating the yield, performing preliminary quality inspection according to United states pharmacopoeia USP43-NF38, and the inspection result is shown in table 3
Table 3 vacuum optimization
| Case (B) | Complexation distillation temperature | Vacuum degree | Yield is good | Purity of | Maximum single impurity |
| Example 4 | 100℃ | 1kpa | 90.2％ | 99.83％ | 0.05％ |
| Example 6 | 110℃ | 1kpa | 90.1％ | 99.85％ | 0.05％ |
| Example 6 | 120℃ | 1kpa | 90.1％ | 99.82％ | 0.07％ |
| Example 7 | 130℃ | 1kpa | 90.2％ | 99.75％ | 0.10％ |
| Example 8 | 140℃ | 1kpa | 90.2％ | 99.51％ | 0.38％ |
From Table 3, it is clear that the temperature of the purification by complexation distillation of stannous oxide is suitably selected to be 100 to 120. The temperature exceeds 120. DegreeC, since stannous oxide itself has a catalytic dehydration effect, new self-condensed impurities are generated.
To further determine the effectiveness of the present application. Experiments were designed to avoid the reduction refining of 1, 3-butanediol and the complex distillation of 1, 3-butanediol acidic impurities, and the results are shown in comparative examples 1 and 2.
Comparative example 1
100g of crude 1, 3-butanediol (purity 99.43%, maximum single impurity 0.23%) is added into a three-neck flask, a thermometer, a condenser tube and the like are arranged, 0.1g of stannous oxide is added, the temperature (100 ℃,110 ℃,120 ℃,130 ℃,140 ℃) and the control pressure are controlled, the vacuum concentration is carried out under the condition that the control pressure is about 1kpa, about 3g of front cut is trapped and concentrated until about 5g of concentrated mother liquor is left, the vacuum concentration is stopped, the temperature is reduced to room temperature, and the 1, 3-butanediol is obtained by sterilization and filtration, and the yield is 90.46%. The purity is 99.56%, the maximum single impurity is 0.17%, and the product is unqualified.
Comparative example 2
100g of crude 1, 3-butanediol (purity 99.43 percent, maximum single impurity of 0.23 percent) is added into a three-neck flask, a thermometer, a condenser tube and the like are arranged, the temperature is controlled to 10-15 ℃, 0.2g of sodium borohydride is slowly added, the temperature is kept and stirred for 0.5h, 1.0g of active carbon is added, the stirring is uniform, and the purified 1, 3-butanediol is obtained after sterilization and filtration, and the yield is 97.46 percent. The content is 99.53 percent, the maximum single impurity is 0.19 percent, and the product is unqualified.
Experiments without carrying out reduction refining on the 1, 3-butanediol and complexation distillation treatment on the 1, 3-butanediol impurity show that the traditional 1, 3-butanediol refining method can remove related substance impurities to reach the limit condition, and the effect that any single impurity is less than 0.1% is difficult to achieve, and only the method can be used effectively. The application successfully develops an effective pharmaceutical grade 1, 3-butanediol refining and purifying method.
In conclusion, the industrial grade or cosmetic grade 1, 3-butanediol is taken as a starting material, refined by a reducing agent, distilled and refined by a complexation protecting agent, and the product is subjected to sterilization and filtration to effectively remove raw material impurities, so that a high-purity medicinal grade 1, 3-butanediol product with less impurities, high purity and light product color and meeting the medicinal requirements is successfully prepared; the refining method has simple process, reasonably utilizes resources, reduces the damage to the environment in the production process, and has strong market competitiveness.
While certain specific embodiments of the application have been described in detail by way of example, it will be appreciated by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the application. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the application. The scope of the application is defined by the appended claims.
Claims (10)
1. A process for preparing pharmaceutical grade 1, 3-butanediol comprising:
mixing industrial-grade 1, 3-butanediol with a reducing agent, stirring for reaction, and performing solid-liquid separation to obtain a reaction solution;
mixing the reaction liquid with a stable complexing agent, heating, distilling under reduced pressure, sterilizing, and filtering to obtain the medicinal 1, 3-butanediol.
2. The process for preparing pharmaceutical grade 1, 3-butanediol according to claim 1, wherein the stirring reaction is carried out at a temperature of-10 to 50 ℃ for a time of 0.5 to 4 hours.
3. The process for preparing pharmaceutical grade 1, 3-butanediol according to claim 2, wherein the stirring reaction is carried out at a temperature of 0 to 5 ℃ for a time of 1-2h.
4. The method of preparing pharmaceutical grade 1, 3-butanediol according to claim 1 wherein the reducing agent comprises sodium borohydride.
5. The method of preparing pharmaceutical grade 1, 3-butanediol according to claim 4 wherein the amount of sodium borohydride is 0.01% -0.5% of the mass of the technical grade 1, 3-butanediol.
6. The method for preparing pharmaceutical grade 1, 3-butanediol according to claim 5 wherein the amount of sodium borohydride is 0.1% of the mass of the technical grade 1, 3-butanediol.
7. The method of preparing pharmaceutical grade 1, 3-butanediol according to claim 1 wherein the stable complexing agent comprises stannous oxide.
8. The method for preparing pharmaceutical grade 1, 3-butanediol according to claim 7 wherein the amount of stannous oxide is 0.05% -0.5% of the mass of the technical grade 1, 3-butanediol.
9. The method for preparing pharmaceutical grade 1, 3-butanediol according to claim 8 wherein the amount of stannous oxide is 0.1% of the mass of the technical grade 1, 3-butanediol.
10. The process for preparing pharmaceutical grade 1, 3-butanediol according to any one of claims 1-9, wherein the reduced pressure distillation is carried out at a temperature of 100-120 ℃ and a vacuum of not more than 5kPa.
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| CN202311015928.2A CN117024251A (en) | 2023-08-14 | 2023-08-14 | Method for preparing medicinal grade 1, 3-butanediol |
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| CN202311015928.2A CN117024251A (en) | 2023-08-14 | 2023-08-14 | Method for preparing medicinal grade 1, 3-butanediol |
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