CN102320932A - Preparation method of 2,3-dihydroxyl methylbenzene - Google Patents

Abstract

The invention discloses a preparation method of 2,3-dihydroxyl methylbenzene. The preparation method comprises the following steps of: adding o-vanillin, potassium hydroxide, hydrazine hydrate and diethylene glycol to a flask, and heating and reacting; then recovering hydrazine hydrate under normal pressure, distilling and insulating heat, then distilling under reduced pressure to recover diethylene glycol, cooling to room temperature, adding water, dropwise adding hydrochloric acid to adjust the pH value to 2-3, extracting with ethyl ether, drying, concentrating, and cooling a residual liquid to room temperature to obtain grey-white solid 2-hydroxyl-3-methyl phenylmethyl ether; and adding 48wt% hydrobromic acid, refluxing, extracting with ethyl ether, drying and distilling under reduced pressure to obtain a finished product. The preparation method disclosed by the invention has the advantages that: the method is simple, the reaction conditions are easy to control, the yield of 2,3-dihydroxyl methylbenzene is high, and the obtained product is a novel chemical substance and has wide applications.

Description

A kind of 2, the preparation method of 3-orcin

Technical field

The present invention relates to a kind ofly 2, the preparation method of 3-orcin belongs to fine chemistry industry compound field.

Background technology

3, the 5-orcin is a white crystals, sees phototropic; Water-soluble and pure, be slightly soluble in benzene, trichloromethane and dithiocarbonic anhydride, keep in Dark Place.3, the 5-orcin mainly is that the cheap 3-methyl-4-chlorophenol of employing is a raw material, makes midbody 3 through high temperature dechlorination hydrolysis single step reaction, the phenol sylvite of 5-orcin, and acidification makes compound then.Also wanting a kind of method to adopt sym-trimethylbenzene be solvent, and tells the water that reaction generates with water trap, at the 164-166 ℃ of about 14h of back flow reaction, can get purity after the processing greater than 98% product, and yield is more than 40%.According to 3, the reaction of 5-orcin can be thought deeply the compound method that other analogues.

Summary of the invention

The object of the present invention is to provide a kind of 2, the preparation method of 3-orcin.

The present invention adopts following technical scheme to achieve these goals:

2, the preparation method of 3-orcin is characterized in that may further comprise the steps:

(1) in flask, adds 74-78g NSC 2150,75-85g Pottasium Hydroxide, 90-110ml Hydrazine Hydrate 80 and 480-520ml glycol ether, be heated to 120-130 ℃, reacted about 3 hours;

(2) normal pressure reclaims Hydrazine Hydrate 80, distills 190-210 ℃, is incubated about 3 hours; Glycol ether is reclaimed in underpressure distillation again, and cool to room temperature adds 280-320ml water; Dripping hydrochloric acid is regulated ph to 2-3, with extracted with diethyl ether 3-4 time, and 190-210ml at every turn; Combining extraction liquid, dry, concentrated, raffinate is cooled to room temperature and gets pale solid 2-hydroxy-3-methyl methyl-phenoxide;

(3) in above-mentioned 2-hydroxy-3-methyl methyl-phenoxide, adding massfraction is 48% Hydrogen bromide 190-210g, backflow 4.5-5.5 hour, and with extracted with diethyl ether 3-4 time, 190-210ml at every turn, drying, underpressure distillation gets finished product.

Beneficial effect of the present invention:

Preparing method of the present invention is simple, easy control of reaction conditions, production cost is low, obtain 2,3-orcin yield is high, and product of the present invention is new chemical substance, applicability is wide.

Embodiment

Embodiment 1:2, the preparation method of 3-orcin may further comprise the steps:

(1) in flask, adds 76g NSC 2150,80g Pottasium Hydroxide, 100ml Hydrazine Hydrate 80 and 500ml glycol ether, be heated to 120-130 ℃, reacted 3 hours;

(2) normal pressure reclaims Hydrazine Hydrate 80, distills to 200 ℃, is incubated 3 hours; Glycol ether is reclaimed in underpressure distillation again, and cool to room temperature adds 300ml water; Dripping hydrochloric acid is regulated ph to 2-3, with extracted with diethyl ether 3 times, and 200ml at every turn; Combining extraction liquid, dry, concentrated, raffinate is cooled to room temperature and gets pale solid 2-hydroxy-3-methyl methyl-phenoxide;

(3) in above-mentioned 2-hydroxy-3-methyl methyl-phenoxide, adding massfraction is 48% Hydrogen bromide 200g, backflow 4.5-5.5 hour, and with extracted with diethyl ether 3 times, 200ml at every turn, drying, underpressure distillation gets finished product 50g.

Claims (1)

1. one kind 2, the preparation method of 3-orcin is characterized in that may further comprise the steps:

(1) in flask, adds 74-78g NSC 2150,75-85g Pottasium Hydroxide, 90-110ml Hydrazine Hydrate 80 and 480-520ml glycol ether, be heated to 120-130 ℃, reacted about 3 hours;

(2) normal pressure reclaims Hydrazine Hydrate 80, distills 190-210 ℃, is incubated about 3 hours; Glycol ether is reclaimed in underpressure distillation again, and cool to room temperature adds 280-320ml water; Dripping hydrochloric acid is regulated ph to 2-3, with extracted with diethyl ether 3-4 time, and 190-210ml at every turn; Combining extraction liquid, dry, concentrated, raffinate is cooled to room temperature and gets pale solid 2-hydroxy-3-methyl methyl-phenoxide;

(3) in above-mentioned 2-hydroxy-3-methyl methyl-phenoxide, adding massfraction is 48% Hydrogen bromide 190-210g, backflow 4.5-5.5 hour, and with extracted with diethyl ether 3-4 time, 190-210ml at every turn, drying, underpressure distillation gets finished product.