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Method for synthesizing compound S-303 hydrochloride

A technology of methyl propionate and amino, which is applied in the field of compound S-303 hydrochloride synthesis, can solve the problems of high equipment requirements, difficulty in cleaning, and great impact on drug quality, and achieve simple operation, cost reduction, and equipment less demanding effect

Inactive Publication Date: 2015-07-22
WUHAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process needs to be carried out in a high vacuum state to remove the solvent and methanol generated in the reaction, which requires high equipment and is not conducive to industrial production
In addition, the reaction uses toluene as a solvent, which is difficult to remove and has a great impact on the quality of medicines

Method used

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  • Method for synthesizing compound S-303 hydrochloride
  • Method for synthesizing compound S-303 hydrochloride

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Experimental program
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Embodiment Construction

[0024] Step 1) Synthesis of S-301 hydrochloride: Add 100 g of 9-chloroacridine to methanol, add 85 g of sodium methoxide, 27.8 g of 3-aminopropionic acid methyl ester hydrochloride, reflux at 68 ° C for 4.5 h, cooled to room temperature, filtered, spin-dried the filtrate, drained the residual solvent with an oil pump, added isopropanol and homogenized at 96°C for 2 hours, cooled to room temperature, filtered to obtain a yellow solid, namely S-301 hydrochloride , The liquid phase detection purity is 96%. 1 H NMR (400MHz, CD 3 OD)δ8.52,8.50,7.99,7.97,7.96,7.95,7.87,7.85,7.59,7.58,7.56,7.56,4.48,4.46,4.45,3.69,3.34,3.33,3.33,3.33,3.32,3.10,3.08, 3.06, 3.04, 3.03.

[0025] Step 2) Synthesis of S-302: 100 g of S-301 was added to 1 L of triethanolamine, and stirred at 35° C. for 40 h. Use 600ml CH 2 Cl 2 The reaction solution was diluted, transferred to a separatory funnel, and saturated with 600 mL of KHCO 3 Solution wash, CH 2 Cl 2 (450mLx3) extracted the aqueous phase, co...

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Abstract

The invention relates to a method for synthesizing a compound S-303 hydrochloride and belongs to the field of organic synthesis. According to the method, S-302 is directly synthesized through taking S-301 hydrochloride as a starting raw material and taking triethanolamine as a reactant and solvent under the condition of not adding any additive, and the reaction conditions are mild. The adoption of a toxic and high-boiling-point solvent, namely toluene, is avoided, and reaction under high-vacuum conditions is avoided, so that the operation is simple, and the requirements on equipment are low; reagents, such as toluene and sodium methoxide, are not used, so that the cost is reduced. Although the reaction time is relatively long, the transformation ratio of S-301 can reach about 83%.

Description

technical field [0001] The invention relates to a synthesis method of compound S-303 hydrochloride, belonging to the field of organic synthesis. Background technique [0002] Blood transfusion is a fast and effective treatment commonly used in clinical practice, but there may be AIDS (HIV), hepatitis B (HBV), hepatitis C (HCV) and other viruses in the blood, so the viruses in the blood must be inactivated to ensure Safety with blood. [0003] At present, the methods of blood virus inactivation can be mainly divided into the following categories: 1) dry heat inactivation virus method, 2) organic solvent combined with surfactant method (S / D method), 3) nanofiltration method, 4) phenothiazine / subunit blue photochemical method, 5) ultraviolet beta propiolactone photochemical method, etc. [0004] The dry heat inactivation virus method cannot completely inactivate HBV, HCV, and HIV, and at the same time, this method has great damage to coagulation factors and other active ingre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D219/10
CPCC07D219/10
Inventor 程双周晖杨健段建利
Owner WUHAN UNIV