Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of 2-hydroxy phenylacetone

A technology of hydroxyphenylbenzene and acetone, applied in the field of pharmaceutical research, can solve the problems of difficult separation, difficult operation, low yield and the like, and achieve the effects of simple processing, short steps and shortened reaction time

Active Publication Date: 2018-05-29
CHANGZHOU RUIMING PHARMA
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, para-isomers are produced during the rearrangement reaction, and the separation is difficult and the yield is low
Expensive catalysts are required for hydrogenation, and the requirements for technical equipment are relatively high, making it difficult to operate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of 2-hydroxy phenylacetone
  • Preparation method of 2-hydroxy phenylacetone
  • Preparation method of 2-hydroxy phenylacetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] in N 2 Under protection, in a 3000ml four-neck flask, add 1500ml dichloroethane, 124g styrene and 122g salicylaldehyde, then add 5mol% PdCl 2 And 5mol% potassium phosphate, heated to 75 ° C for 6.5 hours. Cool down to room temperature, filter with suction, and wash the catalyst with a small amount of dichloroethane. The filtrate was evaporated to dryness to obtain a light yellow viscous liquid. Distilled under reduced pressure to obtain 194 g of a colorless transparent liquid with a yield of 85.8%.

Embodiment 2

[0031] in N 2 Under protection, in a 3000ml four-neck flask, add 1500ml dichloroethane, 124g styrene and 122g salicylaldehyde, then add 2.5mol% PdCl 2 And 2.5mol% potassium phosphate, heated to 75 ° C for 6.5 hours. Cool down to room temperature, filter with suction, and wash the catalyst with a small amount of dichloroethane. The filtrate was evaporated to dryness to obtain a light yellow viscous liquid. Distilled under reduced pressure to obtain 186 g of a colorless transparent liquid with a yield of 82.3%.

Embodiment 3

[0033] in N 2 Under protection, in a 3000ml four-neck flask, add 1500ml dichloroethane, 124g styrene and 122g salicylaldehyde, then add 5mol% PdCl 2 (the seventh recovery) and 5mol% potassium phosphate, the temperature was raised to 75° C. for 6.5 hours. Cool down to room temperature, filter with suction, and wash the catalyst with a small amount of dichloroethane. The filtrate was evaporated to dryness to obtain a light yellow viscous liquid. Distilled under reduced pressure to obtain 189 g of a colorless transparent liquid with a yield of 83.6%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of 2-hydroxy phenylacetone (the formula is shown in the description). The preparation method of the 2-hydroxy phenylacetone particularly comprises the following steps: under the protection of N2, taking styrene and 2-hydroxybenzaldehyde as raw materials, adding an organic solvent, performing coupling reaction in the presence of a noble metal catalyst,adding inorganic salt to serve as an auxiliary catalyst and performing reaction to obtain the 2-hydroxy phenylacetone. The reaction is one-step reaction, the step is short and treatment after reactionis simple; the expensive and rare catalyst is replaced by the common palladium chloride, and industrialization becomes possible; the auxiliary catalyst is added, so that the reaction time is greatlyshortened.

Description

technical field [0001] The invention relates to the field of medical research, in particular to a preparation method of 2-hydroxyphenylpropiophenone. Background technique [0002] Propafenone hydrochloride (propafenone hydrochloride), the chemical name is 1-[2-[2-hydroxy-3-(propylamino)propoxy]phenyl]-3-phenyl-1-propanone hydrochloride, is a German The antiarrhythmic drug developed by Helopharm is a sodium channel blocker class Ic, which was first launched in Germany in 1979 and is mainly used clinically for the prevention and treatment of ventricular or supraventricular ectopic beats, ventricular or supraventricular tachycardia It can also be used to treat ischemic and refractory arrhythmias. [0003] 2-Hydroxyphenylpropiophenone is an important intermediate in the synthesis of propafenone hydrochloride. According to literature reports, the preparation process has the following two kinds. [0004] Method 1: Condensation of diethyl malonate and benzyl chloride, diethyl 2-...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/69C07C49/83
CPCC07C45/69C07C49/83
Inventor 史卫明周禾王小亮
Owner CHANGZHOU RUIMING PHARMA