Heliotropin preparation method

A technology of jasmonal and acetic acid aqueous solution, applied in organic chemistry and other fields

Active Publication Date: 2016-04-20
NORTHEAST PHARMA GRP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sasrole method is the method for producing jasmonal that is adopted by most countries in my country and the world. The characteristic of this method is that it has been used in industry for a long time and is relatively mature in technology. However, the current production of jasmonal More than 90% of raw material sassafras is extracted from sassafras root, so that the resources of sassafras are decreasing day by day, and a large amount of concentrated lye wastewater and sodium dichromate are oxidized to produce jasmonal in the synthesis process. A large amount of chromium-containing wastewater is generated, which seriously pollutes the environment

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  • Heliotropin preparation method

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Experimental program
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Effect test

Embodiment 1

[0015] Add 25ml of glacial acetic acid and 25ml of water into the reaction bottle, start stirring to configure a 50% acetic acid aqueous solution, add urotropine at one time, the amount of urotropine added is shown in Table 1, and when the water bath is cooled to 30°C, add 3 , 4-methylenedioxybenzyl chloride 68g, after the end, keep warm at 10~40°C for 4 hours; add 400ml pure water to the reactant and reflux for 2.5 hours; cool to 30-40°C and extract with chloroform, combine the organic layers to reduce The concentrate was concentrated under reduced pressure, and the concentrate was distilled under reduced pressure, and the fraction with T=85~105°C and P=70~150Pa was collected to obtain white jasmonal crystals. The content and yield are shown in Table 1.

[0016] Table 1: The selection of different addition amounts of urotropine and the content and yield of jasmonal

[0017] serial number Addition of urotropine Molar ratio of 3,4-methylenedioxybenzyl chloride to ...

Embodiment 2

[0019] Add 25ml of glacial acetic acid and 25ml of water into the reaction bottle, start stirring to configure a 50% aqueous solution of acetic acid, add 111.8g of urotropine at one time, and add 3,4-methylenedioxybenzyl dropwise when the water bath is cooled to 30°C Chlorine 68g, keep warm at 10-40°C after the end, see Table 2 for the selection of the holding time; add 400ml pure water to the reactant and reflux for 2.5 hours; cool to 30-40°C and extract with chloroform, combine the organic layers and concentrate under reduced pressure , the concentrate was distilled under reduced pressure, and the fractions with T=85~105°C and P=70~150Pa were collected to obtain white jasmonal crystals. The contents and yields are shown in Table 2.

[0020] Table 2: The selection of different holding times and the content and yield of jasmonal

[0021] serial number Holding time content% Molar yield % 1 2 hours 98.12 69.61 2 3 hours 98.67 72.15 3 4 hours...

Embodiment 3

[0023] Add 25ml of glacial acetic acid and water into the reaction bottle, start stirring to configure an acetic acid aqueous solution, the concentration of the acetic acid aqueous solution is shown in Table 3, add 111.8g of urotropine at one time, and add 3,4-methylene dropwise when the water bath is cooled to 30°C Dioxybenzyl chloride 68g, heat preservation at 10-40°C for 4 hours after the end; add 400ml pure water to the reactant and reflux for 2.5 hours; cool to 30-40°C and extract with chloroform, combine the organic layers and concentrate under reduced pressure, the concentrate Carry out vacuum distillation, collect the distillate of T=85~105 ℃, P=70~150Pa, the content and yield of white jasmonal crystals are shown in Table 3.

[0024] Table 3: the selection situation of acetic acid aqueous solution content and the content and yield of jasmonal

[0025] serial number Acetic acid / water Acetic acid aqueous solution content content% Molar yield % 1 1...

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Abstract

A heliotropin preparation method applied to the chemical synthesis field comprises steps as follows: (1) preparing an acetic acid aqueous solution from glacial acetic acid and water; (2) adding urotropine to the acetic acid aqueous solution once, performing water bath cooling, dropwise adding 3,4-methylenedioxybenzyl chloride, and performing heat preservation after addition; (3) adding pure water to a reactant in Step (2), performing temperature rise reflux, performing cooling after the reaction, extracting the reactant with an organic solvent, mixing organic layers, performing reduced pressure concentration, performing reduced pressure distillation on a concentrate, and collecting heliotropin fractions to obtain heliotropin. The heliotropin prepared with the method is white crystals rather than light yellow crystals containing nitro-compounds. The method has the advantages of simplicity in operation, low energy consumption, low cost, capability of avoiding overexploitation of plant resources and protecting the ecological environment and the like.

Description

Technical field [0001] The present invention involves a method of preparing jasmine aldehyde with 3,4-adetic oxide chlorine as raw materials in the field of chemical synthesis. Background technique [0002] Announcement of jasmine, also known as peppercorns and someware, chemical names are 3,4- (Asian epoxyl) benaldehyde, with white or pale yellow crystals.Anyoneytaldehyde is an important fine chemical and organic synthetic intermediate. It is widely used in food, daily chemical, fine chemicals, medicine and other industries. [0003] At present, the synthesis methods of domestic jasmine aldehyde are mainly: synthetic methods with pepperine as raw materials, and three methods: synthesis method and full synthesis method of the starting raw material with different stacked camphor oil.The synthesis method of peppercorns as the raw material is the earliest preparation method of jasmine aldehyde. This process raw material is rare, the cost is high, and it has been eliminated.The camph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/54
CPCC07D317/54
Inventor 赵晓峰杨会芬王东旭张海宏赵利军李秀媛佟刚符艳妍周中琦王凡
Owner NORTHEAST PHARMA GRP
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