Method for improving clarity of resorcinol

A technology of resorcinol and clarity, applied in the field of medicinal chemistry, can solve problems such as not being able to be used in medicine, not meeting GMP requirements, etc., and achieve the effect of solving the problem of clarity and simple process

Active Publication Date: 2018-11-23
浙江精进药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Resorcinol has a bactericidal effect and can be used as a preservative. It is added to cosmetics and dermatological drug pastes and ointments. As a drug, the production process of resorcinol must comply with the relevant regulations on drug production. Hydroquinone, does not comply with GMP requirements, so it cannot be used medicinally

Method used

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  • Method for improving clarity of resorcinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, a kind of method improving resorcinol clarity,

[0030] Add 75g of commercially available resorcinol (turbidity 33) into 250g of saturated aqueous sodium chloride solution, stir until the resorcinol is dissolved; then add 150g of methyl tert-butyl ether for 2 extractions, and combine the organic phases , add 2g of activated carbon for decolorization, anhydrous sodium sulfate (30g) for dehydration, stir for 1h, filter, concentrate the filtrate at 25°C, vacuum degree ≤ -0.09MPa until no liquid drips out, add 100g of dichloromethane for beating for 1 hour, filter , the solid (filter cake obtained by filtration) was dried to constant weight at 30-40° C. under vacuum (vacuum degree ≤-0.09 MPa) to obtain 50 g of resorcinol (yield 66.7%), and the measured turbidity was 1.3.

Embodiment 2

[0031] Embodiment 2, a kind of method improving resorcinol clarity,

[0032] Add 50g of commercially available resorcinol (turbidity 33) into 150g of saturated aqueous sodium chloride solution, stir until the resorcinol is dissolved; then add 150g of ethyl acetate x 2 extractions, combine the organic phase liquid, add 2g Decolorize with activated carbon, dehydrate with 30g of anhydrous sodium sulfate, stir for 1h, filter, concentrate the filtrate at 25°C, vacuum degree ≤ -0.09MPa until no liquid drips out, add 80g of toluene for beating for 1 hour, filter, solid at 30-40°C Vacuum drying to constant weight yielded 35 g of resorcinol (70% yield), and the measured turbidity was 2.2.

Embodiment 3

[0033] Embodiment 3, a kind of method that improves resorcinol clarity,

[0034] 75 g of resorcinol (turbidity 16) obtained by synthesis was processed according to the method described in Example 1 to obtain 50 g of resorcinol (yield 66.7%) and turbidity 1.2.

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Abstract

The invention discloses a method for improving the clarity of resorcinol. The method comprises the following steps that resorcinol is dissolved through a saturated sodium chloride water solution, anda resorcinol solution is obtained; an organic solvent I is added into the resorcinol solution to conduct extraction; active carbon is added into the organic phase obtained through extraction to conduct decoloration, anhydrous sodium sulfate is utilized to conduct dehydration, and then filtration is conducted; and the obtained filtrate is subjected to vacuum concentration at the temperature of 20-30 DEG C, then an organic solvent II is added to conduct pulping and filtration, a filter cake is dried in vacuum, and resorcinol is obtained. The turbidity of resorcinol obtained by adopting the method can meet the Europe pharmacopoeia criterion.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry. Background technique [0002] Resorcinol is an important pharmaceutical and chemical raw material, mainly used in rubber adhesives, synthetic resins, dyes, preservatives, medicine and analytical reagents, etc. Resorcinol is similar to phenol and cresol, and forms polycondensation with formaldehyde It can be used to make viscose and tire cord binders for nylon, to prepare wood adhesives, and to bond vinyl materials to metals. Resorcinol is an intermediate of many azo dyes and fur dyes , It is also the raw material of p-nitrosalicylic acid, a pharmaceutical intermediate. Resorcinol has a bactericidal effect and can be used as a preservative. It is added to cosmetics and dermatological drug pastes and ointments. As a drug, the production process of resorcinol must comply with the relevant regulations on drug production. Hydroquinone, does not comply with GMP requirements, so it cannot ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/68C07C39/08
CPCC07C37/685C07C39/08
Inventor 许重阳王晖
Owner 浙江精进药业有限公司
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