Synthetic method of prothioconazole midbody 1-chloro-1-acetyl cyclopropane
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of prothioconazole and a synthetic method is applied in the new industrial synthesis field of 1-chloro-1-acetylcyclopropane, can solve the problems of high cost, high price of sodium ethoxide and butyrolactone, and achieves low cost, The effect of high reaction yield and cheap and easy-to-obtain raw materials
Active Publication Date: 2017-01-04
YANGZHOU TIANCHEN FINE CHEM
View PDF4 Cites 13 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0008] In this route, the price of sodium ethoxide and butyrolactone is relatively high, and they are used in the first step reaction, resulting in high overall cost
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
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment Construction
[0038] 1. Production process:
[0039] 1. Synthesis of intermediate compound (2):
[0040] Add compound (1) (223.5g, 1.72 mol) and acetone (1100 ml) into a three-neck round bottom flask, add solid sodium iodide (12.9g, 0.086 mol), 1,2-dichloroethane (681g, 8.88 mol) and anhydrous potassium carbonate (285g, 2.06mol), the temperature was raised to 55°C under the protection of nitrogen, and the stirring was maintained for 24 hours in a slightly boiling reflux state. The gas phase detection reaction showed that the conversion rate of compound (1) was greater than 96%, and the solvent acetone was concentrated and recovered. and dichloroethane, the residue was extracted with tert-butyl methyl ether, filtered, the solid was washed, the filtrate was washed with brine, dried and concentrated, and distilled under high vacuum to obtain 265g of compound (2), the gas phase purity was greater than 97%, and the yield was 80% %.
[0041] 2. Synthesis of intermediate compound (3):
[0042] ...
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
Login to view more
Abstract
The invention relates to a synthetic method of a prothioconazole midbody 1-chloro-1-acetyl cyclopropan, which relates to the technical field of chemical production. The synthetic method comprises the following steps: mixing alkyl acetoacetate and 1,2-dihaloalkane or ethylene glycol disulfonate, performing mono-alkylation reaction, after chloration reaction, mixing with a strong acid, performing hydrolysis, and obtaining 3,5-dichloropentane-2-ketone or 3-chloro-4- sulfonate pentane-2-ketone; and finally taking quaternary ammonium salt as a catalyst, mixing the 3,5-dichloropentane-2-ketone or 3-chloro-4-sulfonate pentane-2-keton and alkali liquor, performing ring closing reaction, and obtaining 1-chloro-1-acetyl cyclopropane. By adopting the synthetic method, the cost is reduced, three wastes (waste water, waste gas and waste residues) are reduced, safety and reliability are realized, and the reaction yield is high.
Description
technical field [0001] The invention relates to the technical field of chemical production, in particular to a new industrial synthesis method of 1-chloro-1-acetylcyclopropane. Background technique [0002] Prothioconazole (common name: prothioconazole) is a new broad-spectrum triazolethione fungicide. Prothioconazole is mainly used to prevent and control many diseases of cereal crops such as wheat, barley, rapeseed, peanut, rice and bean crops. It has a good control effect on almost all wheat diseases, such as powdery mildew, sheath blight, fusarium wilt, leaf spot, rust, sclerotinia, net spot, moire, etc. of wheat and barley. It can also prevent and control soil-borne diseases of rapeseed and peanuts, such as sclerotinia, and major foliar diseases, such as gray mold, black spot, brown spot, black shank, sclerotinia and rust, etc. Good systemic activity, excellent protective, therapeutic and eradicating activities, and long-lasting. Prothioconazole not only has good safe...
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
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.