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

Preparation method of 2, 3-dichloroanisole

A technology of dichloroanisole and dichlorofluorobenzene, which is applied in the field of preparation of 2,3-dichloroanisole, can solve problems such as difficult treatment of high-salt wastewater, impact on product purity, and potential safety hazards, and achieve selectivity High efficiency, less waste, and simple production process

Inactive Publication Date: 2013-03-13
ZHEJIANG DAYANG BIOTECH GROUP
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] This method uses highly poisonous dimethyl sulfate, and its feeding ratio is about 3.5 equivalents of 2,3,-dichlorophenol, and the excessive dimethyl sulfate and by-product sodium monomethyl sulfate are dissolved in the waste water. The reaction not only produces a large amount of wastewater, but also the high-salt wastewater containing the highly toxic dimethyl sulfate is difficult to treat, and it is easy to cause safety hazards in the process of production and wastewater treatment
The purity of the product is 97%~98%, which may have a certain impact on the purity of subsequent products

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, 3-dichloroanisole
  • Preparation method of 2, 3-dichloroanisole
  • Preparation method of 2, 3-dichloroanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of embodiment 1,2,3-dichloroanisole

[0032] Add about 198g of a 30% sodium methoxide methanol solution (containing 1.1mol of sodium methoxide) in a 1000ml three-neck flask equipped with a stirrer, a thermometer and an addition funnel, and add 165g (1mol) of 2,3-dichlorofluorobenzene dropwise at room temperature After 30 minutes, the dropwise addition was completed, and the temperature was raised to 60°C for 10 hours. After the reaction, cool to room temperature, remove the solid by suction filtration, distill the filtrate under reduced pressure, distill methanol off, add 100ml of water and stir thoroughly, precipitate white crystals (white crystals), and filter by suction. Phosphorus oxide was dried in a vacuum oven to constant weight to obtain 174.2 g of the product 2,3-dichloroanisole, Y (yield) = 98.4%, content (GC detection) ≥ 99%.

Embodiment 2

[0033] The preparation method of embodiment 2,2,3-dichloroanisole

[0034] Add 360g of 30% sodium methoxide methanol solution (containing 2.0mol of sodium methoxide) in a 1000ml three-necked flask equipped with a stirrer, a thermometer and an addition funnel, and add 165g (1mol) of 2,3-dichlorofluorobenzene dropwise at room temperature. The dropwise addition was completed in 30 minutes, and the temperature was raised to 80° C. for 2 hours. After the reaction was finished, cool to room temperature, remove the solid by suction filtration, distill the filtrate under reduced pressure, steam methanol, add 200ml of water and stir thoroughly, and white crystals were precipitated, filtered by suction, and the white crystals obtained by suction filtration were mixed with phosphorus pentoxide. Dry in a vacuum drying oven to constant weight to obtain 173.6 g of the product 2,3-dichloroanisole, Y (yield) = 98.1%, content (GC detection) ≥ 99%.

Embodiment 3

[0035] The preparation method of embodiment 3,2,3-dichloroanisole

[0036] Add 600g of 10% sodium methoxide methanol solution (containing 1.11mol of sodium methoxide) in a 1000ml three-necked flask equipped with a stirrer, thermometer and addition funnel, and add 165g (1mol) of 2,3-dichlorofluorobenzene dropwise at room temperature. The dropwise addition was completed in 30 minutes, and the reaction was incubated at 20° C. for 24 hours. After the reaction is finished, cool to room temperature, remove the solid by suction filtration, distill the filtrate under reduced pressure, steam methanol, add 100ml of water and stir thoroughly, and white crystals are precipitated, filtered by suction, and the white crystals obtained by suction filtration are mixed with phosphorus pentoxide. Dry to constant weight in a vacuum drying oven to obtain 170.9 g of the product, Y (yield) = 96.6%, content (GC detection) ≥ 99%.

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 discloses a preparation method of 2, 3-dichloroanisole. The preparation method adopts 2, 3-dichlor fluorbenzene as a raw material and sequentially comprises the following steps: 1) reacting 2, 3-dichlor fluorbenzene with a methanol solution of sodium methylate at the temperature of 20-80 DEG C for 2-24h, wherein the molar ratio of sodium methylate in the methanol solution of sodium methylate to 2, 3-dichlor fluorbenzene is 1-4: 1; and 2) cooling a product obtained in the step 1), then filtering, performing decompression distillation on obtained filtrate to recover methanol, further adding water for stirring treatment, and performing drying treatment on a precipitated white crystal to get the 2, 3-dichloroanisole. The method disclosed by the invention is adopted for preparing 2, 3-dichloroanisole, is in line with the concept of green chemistry and has the characteristic of high yield.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a preparation method of 2,3-dichloroanisole. Background technique [0002] 2,3-Dichloroanisole is a key intermediate in the preparation of a diuretic, diuretic acid (also known as ethacrynic acid). Diuretic acid is a powerful and rapid diuretic drug; it is quickly absorbed after oral administration, and the urine output begins to increase within 30 minutes, and reaches the peak within 2 hours, and the drug effect lasts for about 6 to 8 hours; it starts 5 to 10 minutes after intravenous injection Diuretic, peaking in 1 to 2 hours, the effect can be maintained for 2 hours. Mainly used for the treatment of: heart failure, acute pulmonary edema, edema caused by kidney disease, liver disease ascites, schistosomiasis ascites, cerebral edema and other diseases. It is the most widely used diuretic at present. [0003] The method for preparing 2,3-dichloroanisole of bibliographical report...

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
IPC IPC(8): C07C43/225C07C41/16
Inventor 徐旭辉王国平王丽佳
Owner ZHEJIANG DAYANG BIOTECH GROUP