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Preparation method of SPDIB

A dripping and filter cake technology, applied in the field of biomedicine, to achieve the effect of low raw material cost and short steps

Inactive Publication Date: 2020-04-14
苏州络森生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Also there is no report about this alkaloid synthesis method in the prior art

Method used

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  • Preparation method of SPDIB
  • Preparation method of SPDIB

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preparation example Construction

[0017] A kind of preparation method of SPDIB of the present invention, comprises the steps:

[0018] ① Dissolve 2,3,3-trimethyl-3H-indole in toluene, add 1,3-propane sultone dropwise, heat up to 120°C for reflux reaction for 4-5 hours after dropping, then cool to room temperature, Filter to obtain filter cake;

[0019] ② recrystallize the filter cake obtained in step ① to obtain light yellow powder;

[0020] ③Co-dissolve the light yellow powder obtained in step ② with 3,5-diiodo-4-hydroxybenzaldehyde in absolute ethanol, add pyridine dropwise under the protection of nitrogen, and heat up to 80°C to react for 7-8 hours after dropping. The resulting reaction solution was concentrated under reduced pressure to leave a residue;

[0021] ④ acidify the residue obtained in step ③ to pH 2.0 with hydrochloric acid, allow the oily product to separate out, extract with ethyl acetate, and combine the extracts;

[0022] ⑤Elute the extract obtained in step ④ with methanol and dichloromet...

Embodiment 1

[0028] Add 138g (0.87mol) of 2,3,3-trimethyl-3H-indole and 600ml of toluene into a 1000ml three-necked flask, stir until the solid dissolves, add dropwise 106g (0.87mol) of 1,3-propane sultone , the temperature was raised to 120° C. for reflux reaction for 4 hours after dropping, and the reaction was confirmed to be complete. Cool to room temperature, filter, and recrystallize the filter cake with methanol to obtain 191 g of light yellow powder (main component 2,3,3-trimethyl-1-(3-sulfonic acid propyl)-3h-indole).

[0029] In a 2000ml three-neck flask, first add 191g (0.68mol) of light yellow powder, 196g (0.52mol) of 3,5-diiodo-4-hydroxybenzaldehyde, 1500ml of absolute ethanol, stir, and add pyridine dropwise under nitrogen protection. 41g (0.52mol), after dripping, heat up to 80°C and react for 8 hours. After the reaction is over, concentrate under reduced pressure to remove the solvent. The residue is acidified to PH2.0 with 5% hydrochloric acid, and an oily product is prec...

Embodiment 2

[0031] Add 138g (0.87mol) of 2,3,3-trimethyl-3H-indole and 600ml of toluene into a 1000ml three-necked flask, stir until the solid dissolves, add dropwise 106g (0.87mol) of 1,3-propane sultone , the temperature was raised to 120° C. for reflux reaction for 4.5 hours after dropping, and the reaction was confirmed to be complete. Cool to room temperature, filter, and recrystallize the filter cake with methanol to obtain 187 g of light yellow powder (main component 2,3,3-trimethyl-1-(3-sulfonic acid propyl)-3h-indole).

[0032] In a 2000ml three-necked flask, first add 187g (0.67mol) of light yellow powder, 196g (0.52mol) of 3,5-diiodo-4-hydroxybenzaldehyde, 1500ml of absolute ethanol, stir, and add pyridine dropwise under nitrogen protection. 41g (0.52mol), after dropping, heat up to 80°C and react for 7.5 hours. After the reaction is over, concentrate under reduced pressure to remove the solvent. The residue is acidified to PH2.0 with 5% hydrochloric acid. An oily product is pr...

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Abstract

The invention belongs to the technical field of biological medicines, and relates to an SPDIB preparation method, which comprises: (1) dissolving 2,3,3-trimethyl-3H-indole in toluene, adding 1,3-propane sultone in a dropwise manner, heating to a temperature of 120 DEG C after the addition, carrying out a reflux reaction for 4-5 h, cooling to a room temperature, and filtering to obtain a filter cake; (2) re-crystallizing the filter cake to obtain faint yellow powder; (3) co-dissolving the faint yellow powder and 3,5-diiodo-4-hydroxybenzaldehyde in absolute ethyl alcohol, adding pyridine in a dropwise manner, heating to 80 DEG C after adding, reacting for 7-8 hours, and concentrating the reaction solution under reduced pressure to obtain residues; (4) adding hydrochloric acid into the residues, acidifying until the pH value is 2.0, extracting by using ethyl acetate, and combining the extracting solution; and (5) carrying out gradient elution on the extracting solution in a chromatographic column to obtain SPDIB crystal powder. According to the new preparation method of the SPDIB, the adopted raw materials are low in cost, the step number of the preparation route is short, the yield can reach more than 37%, and the new preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of biomedicine, in particular to a preparation method of SPDIB. Background technique [0002] SPDIB is the main substrate of urinalysis test strips. Urinalysis test strips can quickly detect urobilinogen (URO), bilirubin (BIL), ketone body (KET), blood (BLD), protein (PRO), glucose (GLU), pH value, nitrous acid (NIT) , specific gravity (SG), leukocyte (LEU) and other biochemical indicators. The sensitivity, accuracy, stability, and anti-interference performance of analytical test paper have a lot to do with whether high-quality stabilizers, color developers and other raw and auxiliary materials are used. As a new alkaloid, SPDIB has better sensitivity, accuracy, stability and anti-interference than the existing urine test paper substrate. [0003] SPDIB(3H-Indolium,2-[2-(4-hydroxy-3,5-diiodophenyl)ethenyl]-3,3-diMethyl-1-(3-sulfopropyl)-inner salt, 2-[2-(4- Hydroxy-3,5-diiodophenyl)vinyl]-3,3-dimethyl-1-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/12
CPCC07D209/12
Inventor 陆林林
Owner 苏州络森生物科技有限公司
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