Diosmin | Aryl Hydrocarbon Receptor Agonist

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Quality Control of Diosmin Purity: 95% SDS Specification

COA

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NMR

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Product Details of Diosmin

CAS No. :	520-27-4
Formula :	C₂₈H₃₂O₁₅
M.W :	608.54
SMILES Code :	O=C1C=C(C2=CC=C(OC)C(O)=C2)OC3=CC(O[C@H]4[C@@H]([C@H]([C@@H]([C@@H](CO[C@H]5[C@@H]([C@@H]([C@H]([C@H](C)O5)O)O)O)O4)O)O)O)=CC(O)=C13
Synonyms :	3’,5,7-Trihydroxy-4’-methoxyflavone 7-rutinoside
MDL No. :	MFCD00009772
InChI Key :	GZSOSUNBTXMUFQ-YFAPSIMESA-N
Pubchem ID :	5281613

Safety of Diosmin

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H315-H319-H335
Precautionary Statements:	P261-P305+P351+P338

Application In Synthesis of Diosmin

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

Downstream synthetic route of [ 520-27-4 ]

[ 520-27-4 ] Synthesis Path-Downstream 1~35

1
[ 520-26-3 ]
[ 520-27-4 ]

Yield	Reaction Conditions	Operation in experiment
85.7%	With morpholine; iodine; at 40 - 70℃;Large scale; Green chemistry;	In 20L reaction kettle, add hesperidin 2 kg, iodine 0.92 kg, then add morpholine 12L. Start stirring and elevating temperature. When the temperature rises to 40 deg.C, sample is completely dissolved, At 45 deg.C ± 5 deg.C maintain temperature for 0.5 hours.Then, increase the temperature to 70 deg.C ± 5 deg.C and maintain the temperature and stir for 1.5-3 hours (HPLC monitoring hesperdin completely after transformation as the end point of the reaction). Recovery solvent to reactant into a viscous, adding 12L purified water, stirring, the material after being homogenized, the hydraulic the reaction buffer tank, adding hydrochloric acid adjusting pH=5-7 to crystallization, filtration, filter cake and filtrate, the filtrate pH=2 adjusted by adding hydrochloric acid, slowly adding 30% hydrogen peroxide 0.41 kg, filter, recovery elemental iodine. The filter cake is washed with a large amount of water washing, diosmin mode crude product obtained. Dissolving the purified water is added to the purification tank 12L and 0.39 kg sodium hydroxide, stir until completely dissolved after diosmin mode crude product into the continue to stir until completely dissolved, slowly adding at 20L acetonitrile, the solid is separated out, filtering, takes filters cake (diosmin mode sodium salt purity is of 99.27%), again dissolving the purified water is added to the purification tank 30L, then add and stir the filter cake to be completely dissolved, slowly dilute hydrochloric acid in this case adjusting pH=5-7, a large number of solid precipitation, filtration, the filter cake is washed with a large amount of purified water washing 1 hours, collecting filter cake, is put into the 80 C ± 5 C blast drying, crushing, diosmin mode the finished product to 1.69 kg, the purity is 99.44%, the yield is 85.7%, to the solvent recovery rate 80.1%, iodine recovery rate 89.6%, residual solvent, -related impurities are standard.
	With pyridine; iodine; sodium hydroxide; at 95 - 105℃;Product distribution / selectivity;	100 gm of hesperidin , 700 ml of recovered pyridine, 9.8 gm of sodium hydroxide and 45.6 gm of iodine were charged in 2 liter clean glass assembly . The resulting solution was heated to 95-1050C for 9 - 10 hrs. Reaction was monitored by HPLC. Pyridine was recovered completely by distillation. Charged methanol to the resulting solid, the reaction mass was heated to reflux and filtered at room temperature. The solid obtained was treated with sodium thiosulfate solution and 900 ml, 5% aqueous NaOH solution. pH 2-4 was adjusted with cone, sulfuric acid. Reaction mass was filtered to obtain crude diosmin. Crude diosmin obtained was 80 - 86 gm. Purity was 98.6 %.
13.1 g		Take an amount of 95% hesperidin 20g (previously 90 dried 3-4h), DMSO50ml dissolved by heating, the other to take 3gKBH4, graded by adding, to the reduction of hesperidin naringin type flavan-4- alcohol completely (approximately overnight , UV monitor, under alkaline conditions scans at no absorption peak at 360nm).Slowly adding 5ml of concentrated sulfuric acid (2ml particularly slow first, the solution became light red), mix well (solution becomes light red) was added slowly added anhydrous n-amyl alcohol 120ml, precipitation sink to the bottom, still 30min, poured out positive amyl alcohol solution was added to the precipitate in anhydrous n-amyl alcohol 20ml, stirring rapidly pinching solution, n-amyl alcohol was decanted, treated twice with the law, anhydrous pyridine 40ml, by adding iodine 8.3g, and stir until dissolved, no calcium sulfate 5g, stir, sealed in a water bath at 55 96h after continuous reaction.Activated carbon was added 5.0, add water 500ml, stirring slowly adding phosphoric acid modulation pH5, filtration, the filtrate was adsorbed by 300gD101 macroporous resin, 500ml water to remove pyridine, iodine ions and other impurities, and then 0.1% 0.5% phosphoric acid vitamin C400ml further elution remove residual iodine, pyridine and other impurities, washed with water 300ml, 2000ml eluted with 60% ethanol, recovering ethanol under reduced pressure.After recovery of ethanol was combined with activated charcoal 2g, mixing, filtration, water was recovered under reduced pressure to dryness to obtain Diosmetinidin-7-O-rutinoside, orange powder 13.1 g.

93 kg	With bromine; iodine; In N,N-dimethyl-formamide; at 90 - 120℃;Large scale;	in a 500kg of reactor, added 300.0kg of DMF, slowly added 100. 0kg of hesperidin, then added iodine1.0~5.0kg and bromine 1.0~3.0kg, while stirring the reaction was slowly heated to 90~120 C and at this temperature keep the reaction for 12~16h. The content of diosmin was detected by the sample. When the content of hesperidin was less than 1.0% then stop the reaction. Filtration, the filtrate at 80 ~ 95 C and under the vacuum is - (0.05 ~ .07) Mpa carried out recovery of solvent, to obtain creamy diosmin . in the paste creamy diosmin added 1200kg of purified water, stirred properly , stir, heated up to 40 ~ 70 C and maintain this temperature for 30 ~ 60min, Pressure filtration and wash until the outflow of water is clear. The filter cake dried in the drying room to moisture 8 ~ 15% to obtain crude product 108kg. The crude product was put into the reactor, added 864kg, 648kg and 432kg of 85% ethanol respectively, and then adding 400kg of iodine removing agent, stirring and refluxing for 60min, 40min and 30min respectively. Pressure filtration and wash until the outflow of water is clear. The filter cake was put into a reaction kettle, 700 kg of purified water, stirred properly until became thin paste, with hydrochloric acid, sulfuric acid or acetic acid PH as adjusted to 5, boiled for 40min, Pressure filtration, washing to the outflow of water until was neutral, filter cake was flash Dried to obtain 93 kg of the dried product, then granulated with a micropowder machine to obtain the diosmin according to EU EP 8.0.
	With pyridine; iodine; at 100℃; for 12h;Large scale;	300 kg of liquid phase content of 95%New hesperidin, 1800 kg pyridine, 240 kg iodine into 3000 litersIn the kettle, the temperature is raised to 100 C for 12 hours, the liquid phase monitors the new hesperidin content to less than 2%, and the pyridine is recovered under reduced pressure to no liquid.After the body is steamed, the new odisamine is obtained

References: [1]Archiv der Pharmazie,1983,vol. 316,p. 219 - 222.
[2]Patent: CN105732744,2016,A .Location in patent: Paragraph 0040; 0041.
[3]Proceedings - Indian Academy of Sciences, Section A,1949,p. 151,157.
[4]Patent: WO2010/92592,2010,A2 .Location in patent: Page/Page column 9; 10.
[5]Patent: CN105481918,2016,A .Location in patent: Paragraph 0025.
[6]Patent: CN103435666,2016,B .Location in patent: Paragraph 0016.
[7]ChemBioChem,2019,vol. 20,p. 210 - 220.
[8]Patent: CN109180627,2019,A .Location in patent: Paragraph 0027-0030; 0035-0038; 0043-0046; 0051-0054.

2
[ 69081-76-1 ]
[ 520-27-4 ]

References: [1]Chemische Berichte,1943,vol. 76,p. 452,457.

3
hesperidin octaacetate [ No CAS ]
[ 520-27-4 ]

References: [1]Phytochemistry,1981,vol. 20,p. 297 - 304.

4
[ 108-24-7 ]
[ 520-27-4 ]
diosmetin 7-rutinoside octaacetate [ No CAS ]

References: [1]Phytochemistry,1981,vol. 20,p. 297 - 304.

5
[ 520-27-4 ]
[ 520-34-3 ]

Yield	Reaction Conditions	Operation in experiment
85%	With sulfuric acid; water; at 20℃; for 0.166667h;	General procedure: Sulfuric acid (2.0mL, 0.037mmol) was added dropwise to a beaker (100 mL) containing scutellarin (50 mg, 0.11 mmol). It was shaken or agitated by ultrasound agitated to dissolve the substrate in the acid at room temperature. Water (2.0 mL) was then added carefully dropwise. When the evolution of heat ceased (in 10 minutes), the mixture was added to water (15 mL) in one portion with stirring with a glass rod. The yellow crystals that were deposited were collected by suction filtration and washed by water (5 mL). In most cases, such products were pure enough for direct use. Moreover, it could be further purified by recrystallisation from aqueous methanol (70%, v/v) or column chromatography on silica gel (eluent:ethyl acetate/formic acid/water=100/4/3, v/v/v, Rfs of SCU and SCUE were 0.1 and 0.8 on silica gel GF254 respectively). Light yellow crystals were obtained after recrystallisation (28.5mg, 93% yield); m.p. 285-287C (>300C)27. IR (KBr, cm-1): numax 3442, 3331, 3098, 1671, 1619, 1587, 1509. 1H NMR (500MHz, DMSO-d6): delta 12.80 (s, 1H, 5-OH), 10.48 (s, 1H, 7-OH), 10.33 (s, 1H, 4?-OH), 8.75 (s, 1H, 6-OH), 7.92 (d, 2H, J=8.6Hz, C2?, C6?-H), 6.92 (d, 2H, J=8.6Hz, C3?, C5?-H), 6.75 (s, 1H, C3-H), 6.58 (s, 1H, C8-H). HR-ESI-MS (m/z): 309.0363 for [M+Na]+, calcd 309.0370.
100 kg	With sodium hydroxide; at 100℃; for 0.666667h;Large scale;	Add to the new dioxin obtained in step 1)1500 kg of sodium hydroxide solution with a mass concentration of 32%, continue to raise the temperature to 100 C for 40 minutes, and after monitoring the content of neodoxime to 2% or less in the liquid phase, add hydrochloric acid to the reaction solution to neutralize the pH to 6 7, then cool down to 15 C ~ 25 C to cool, centrifuge, collect the precipitate, and wash the precipitate,Get 120 kg of geranyl lignin crude; Step 3) Preparation of geranyl ligninAdd 20 times volume of ethanol with a mass concentration of 80% to 120 kg of crude geranin, and heat to reflux.Solution, then add 12 kg of activated carbon for decolorization. After the decolorization is completed, the activated carbon is removed by filtration, the filtrate is collected, and the filtrate is concentrated under reduced pressure to 1/3 of the original volume using a double-effect concentrator. The solution is allowed to stand, cooled and crystallized, and centrifuged to obtain geranium lignin. Boutique 100 kg.

References: [1]Journal of Medicinal Chemistry,2011,vol. 54,p. 95 - 106.
[2]Journal of Chemical Research,2014,vol. 38,p. 396 - 398.
[3]Polish Journal of Chemistry,1983,vol. 57,p. 1283 - 1286.
[4]Patent: CN109180627,2019,A .Location in patent: Paragraph 0027; 0031-0034; 0035; 0039-0042; 0043; 0047-0050.

6
[ 520-27-4 ]
[ 107-07-3 ]
[ 80604-68-8 ]

Yield	Reaction Conditions	Operation in experiment
	With triethylamine; In methanol; under 0.45 - 0.5 Torr;Large scale;	The measurement of accurate 240.0kg methanol vacuum into the reactor, from the reactor mouth slowly added to the Austen Siming 60.0kg, triethylamine 1.0kg, the measurement of accurate 2-chloroethanol 22.5kg added to the reactor, open The autoclave heats the steam valve so that the pressure inside the kettle is kept at 0.45 ~ 0.50MPa for 1.0 ~ 3.0h. In the course of the reaction, the pressure is measured after the sampling test, otherwise the reaction continues until the qualified.Add 2.5 kg of activated charcoal to the decolorizer for 30 min.The bleach solution is filtered to the storage tank by hot pressing.From the storage tank to filter the good material to the crystallization tank on the crystallization of the cylinder, the water temperature is not higher than 30 , with concentrated hydrochloric acid to adjust the pH value of 3 to 4, crystallization 24 ~ 48h after centrifugation.

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.
[2]Patent: CN103601773,2016,B .Location in patent: Paragraph 0024-0026.

7
[ 520-27-4 ]
[ 107-07-3 ]
[ 80604-69-9 ]

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.

Yield	Reaction Conditions	Operation in experiment
		Specifically preferred are compounds selected the group of: Flavone, Baicalein, Diosmin, Kaempferide Tangeretine, 3-OH-Flavone Fisetin, Myricetin, Flavanone, ...

9
(S)-5-acetoxy-2-<3-acetoxy-4-methoxy-phenyl>-7-<O²,O³,O⁴-triacetyl-O⁶-(tri-O-acetyl-α-L-rhamnopyranosyl)-β-D-glucopyranosyloxy>-chroman-4-one [ No CAS ]
[ 520-27-4 ]

References: [1]Journal of Organic Chemistry,1951,vol. 16,p. 930,931.

10
5-hydroxyheptaacetyldiosmin [ No CAS ]
[ 520-27-4 ]

References: [1]Tetrahedron Letters,2005,vol. 46,p. 4341 - 4343.

11
[ 108-24-7 ]
[ 520-27-4 ]
[ 6195-54-6 ]

Yield	Reaction Conditions	Operation in experiment
62%	With sodium fluoride; at 130℃; for 0.583333h;Microwave irradiation;	Diosmin (2, 0.05 g, 0.08 mmol) and NaF (0.42 g, 10 mmol) were mixed in acetic anhydride (4 mL) and the mixture was kept under MW irradiation (400 W) at 130 C, for 35 min. After cooling, the solution obtained was poured into ice and then extracted with CH2Cl2. The organic layer was extracted with NaHCO3 followed by crystallization from MeOH/H2O provided 5,3-O-acetyl-2-(3-O-acetyl-4-methoxyphenyl)-7-[2,3,4-tri-O-acetyl-alpha-L-rhamnopyranosyl-(16)-2,3,4-tri-O-acetyl-beta-D-glucopyranosyloxy] oxychromen-4-one (6) as a yellow solid (0.048 g, 0.051 mmol, 62 % yield); mp 135-138 C.

References: [1]Tetrahedron,2006,vol. 62,p. 4038 - 4051.
[2]Molecules,2018,vol. 23.
[3]ChemBioChem,2019,vol. 20,p. 210 - 220.

12
[ 14210-25-4 ]
[ 520-27-4 ]
[ 771480-96-7 ]

References: [1]Journal of Natural Products,2004,vol. 67,p. 1624 - 1627.

13
[ 520-27-4 ]
[ 50848-66-3 ]

References: [1]Journal of Natural Products,2004,vol. 67,p. 1624 - 1627.

14
[ 520-27-4 ]
[ 480-44-4 ]

References: [1]Journal of Natural Products,2004,vol. 67,p. 1624 - 1627.

15
[ 520-27-4 ]
[ 5128-44-9 ]

References: [1]Journal of Natural Products,2004,vol. 67,p. 1624 - 1627.

16
[ 520-27-4 ]
[ 480-36-4 ]

References: [1]Journal of Natural Products,2004,vol. 67,p. 1624 - 1627.

17
[ 520-27-4 ]
5,7-Dihydroxy-2-[3-(2-hydroxy-ethoxy)-4-methoxy-phenyl]-chromen-4-one [ No CAS ]

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.

18
[ 520-27-4 ]
7-Hydroxy-5-(2-hydroxy-ethoxy)-2-[3-(2-hydroxy-ethoxy)-4-methoxy-phenyl]-chromen-4-one [ No CAS ]

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.

19
[ 520-27-4 ]
[ 172805-77-5 ]

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.

20
[ 520-27-4 ]
5,7-Bis-(2-hydroxy-ethoxy)-2-[3-(2-hydroxy-ethoxy)-4-methoxy-phenyl]-chromen-4-one [ No CAS ]

References: [1]Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry,1996,vol. 35,p. 19 - 22.

Yield	Reaction Conditions	Operation in experiment
	In N,N-dimethyl-formamide; at 90 - 95℃;Purification / work up;	100 gm of crude <strong>[520-27-4]diosmin</strong> as prepared in example 1 and 1800 ml of dimethylformamide was charged in 3 liter clean glass assembly. The resulting mass was heated to 90-950C to obtain clear solution. 200 ml of water was added at 90- 950C and maintained for 30 min. The reaction mass was cooled and filtered. The wet solid was collected.Charged wet solid obtained in 3 liter clean glass assembly and charged 900 ml of water, 900 ml of 5% aqueous NaOH solution. Distilled out approximately 900 ml of water under vacuum below 5O0C. Charged 1000 ml of water and the resulting reaction mass was treated with charcoal and filtered through hyflow. pH 1.8-2.2 was adjusted using sulfuric acid. Stirred the mass for 30 min, filtered and washed it with water, hot water. Solid was dried. Yield : 80 - 85 gm. Assay : 99.9 %.

22
[ 520-27-4 ]
diosmin 2'',2''',3'',3''',4'',4'''-O-hexasulfate [ No CAS ]

References: [1]Journal of Medicinal Chemistry,2011,vol. 54,p. 95 - 106.

23
[ 520-27-4 ]
[ 7585-39-9 ]
C₂₈H₃₂O₁₅*C₄₂H₇₀O₃₅ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	In ethanol; water; for 2h;Milling;	The required amounts of the DIOS:beta-CD in themolar ratio of 1:1 and1% w/w PEG 6000 were weighed accurately following the abovedescribed phase solubility study procedure. The homogenous pastes ofbeta-CD and beta-CD-/PEG were prepared in a mortar by adding water:ethanol mixture (1:1) in small quantities for binary and ternarysystems, respectively. The required amount of DIOS powder was thenadded to these pastes with continuous kneading for 2 h. An appropriateamount of water:ethanol mixture (1:1) was added further to maintainthe suitable consistency of the paste. These were dried in a hot airoven at 40-50 C for 4 h. The dried complexes were then powderedand passed through sieve No. 44 and stored in airtight containers tillfurther use.

References: [1]Journal of Molecular Liquids,2014,vol. 199,p. 35 - 41.

24
[ 520-27-4 ]
diosmetinidin [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
1.73 g	With hydrogenchloride; In ethanol; water; at 160℃; for 10h;	Example 3 taken Diosmetinidin-7-O-rutinoside sample 5g, 10% hydrochloric acid was added to 20% ethanol solution 100ml60 10H hydrolysis, water was added 100ml, D101120g macroporous adsorption resin, washed with water 500ml impurity, washed with 75% ethanol 1500ml off, vacuum decompression recovery of ethanol, derived Diosmetinidin, orange powder was 1.73 g.

References: [1]Patent: CN105481918,2016,A .Location in patent: Paragraph 0026.

25
vanadyl(IV) chloride [ No CAS ]
[ 7732-18-5 ]
[ 520-27-4 ]
[ 1310-73-2 ]
[VO(dios)(OH)₃]Na₅*6H₂O [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	pH 12;	Diosmin (1 mmol) was dissolved in an aqueous solution(20 mL) by the addition of a concentrated NaOH solution up to pH 12. A 50% aqueous solution of VOCl2 (0.5 mmol) was addedwith stirring and green solution was formed. Then, a green solidcomplex was precipitated with isopropyl alcohol. The solid was filteredand washed several times with cold isopropyl alcohol andair-dried. Anal. Calcd for C28H43O25VNa5: C, 35.5; H, 4.5; V, 5.4;Na, 12.2. Exp.: C, 35.3; H, 4.4; V, 5.5; Na, 12.2. UV-vis data for1:1 V(IV)O2+ to <strong>[520-27-4]diosmin</strong> ratio, pH 12, kmax (DMSO): 562 nm and665 nm. Thermal analysis (TGA) (oxygen atmosphere, 50 mL/min): in the first step (20-200 C) six water molecules are lost(11.4%). The dehydrated product rendered Na3VO4 (characterizedby infrared spectroscopy) and Na2O at 800 C. The weight of thefinal residue was 26.0%, in agreement with the theoretical value.Diffuse reflectance spectrum: 700 nm.

References: [1]Bioorganic and Medicinal Chemistry,2016,vol. 24,p. 4108 - 4119.

26
C₃₀H₃₄O₁₆ [ No CAS ]
[ 520-27-4 ]

Yield	Reaction Conditions	Operation in experiment
	With water; sodium hydroxide; for 1.5h;	The reaction mixture is added to a vessel containing aqueous NaOH solution (1200 mL, 2.0-2.5 M) and the mixture is kept for 90 minutes, and then sulphuric acid is added until reaching a pH of 7.5. The precipitate is then filtered and washed with water, to obtain wet crude diosmin. The crude diosmin thus obtained is crystallized by dissolving it in aqueous NaOH solution, and subsequently acidifying with sulphuric acid until product precipitation. The solid is filtered, washed with water and dried. 92 g of diosmin were obtained (77% yield). Purity 90% HPLC. The iodine content was 750 ppm as determined by a potentiometry assay after oxygen combustion, according to the methods 2.2.36 (Potentiometric determination of ionic concentration using ion-selective electrodes) and 2.5.10 (Oxygen-flask method) disclosed in the European Pharmacopoeia 8.3 Edition.

References: [1]Patent: WO2016/124585,2016,A1 .Location in patent: Page/Page column 18.

27
[ 64726-90-5 ]
[ 520-27-4 ]

References: [1]Patent: WO2016/124585,2016,A1 .

28
C₃₀H₃₆O₁₆ [ No CAS ]
[ 520-27-4 ]

References: [1]Patent: WO2016/124585,2016,A1 .

29
[ 75-21-8 ]
[ 520-27-4 ]
5-(2-Hydroxy-ethoxy)-2-(3-hydroxy-4-methoxy-phenyl)-7-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-((2R,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyl-tetrahydro-pyran-2-yloxymethyl)-tetrahydro-pyran-2-yloxy]-chromen-4-one [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With pyridine; In methanol; under 2850.29 - 3750.38 Torr;Sealed tube; Large scale;	Closed a good reactor mouth, the measurement of accurate 120.0kg methanol vacuum into the reactor, open the reactor mouth, start stirring, slowly from the reactor mouth to join the Austin 30.0kg, 0.5kg pyridine, sealed reactor mouth, Accurate measurement of ethylene oxide 8.5kg Vacuum into the reactor, open the reactor Heat steam valve heating, to be on the reactor pressure gauge to 0.38MPa pressure to close the steam carotast valve, until the pressure rose to 0.45MPa Time, so that the pressure inside the kettle in the 0.45 ~ 0.50Mpa, to maintain 1.0 ~ 3.0h (in the process if the pressure drop close to 0.45MPa when the need to open the hot steam valve pressure, the pressure rise close to 0.45MPa need to use cooling water ), After the reaction for 1.0h from the sampling port, the reaction solution is clear and transparent, good mobility, thin-layer chromatography after testing began to buck, otherwise, continue to respond until the test qualified.Once every 5min record pressure, the pressure dropped to 0.12 ~ 0.14MPa when the reaction liquid into the decolorization tank.

References: [1]Patent: CN103601773,2016,B .Location in patent: Paragraph 0020-0023.

30
[ 520-27-4 ]
[ 2174-59-6 ]