Tech. for synthetic (4-chlorobutyl) 1-cyclohexyl-1,2,3,4-tetrazole
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A production process, cyclohexyl technology, applied in the direction of organic chemistry, can solve the problems of hydrogen chloride pollution, high price, prone to explosion production accidents, etc., and achieve the effect of not being prone to accidents, not easy to decompose or volatilize
Inactive Publication Date: 2006-06-28
许建强
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[0006] 1. The raw material valerolactone needs to be imported, and the price is too high
[0007] 2. The amount of phosphorus pentachloride required in the reaction process from (A) to (B) is relatively large, and the hydrogen chloride discharged is likely to cause pollution
[0008] 3. Hydrogen azide is a highly toxic chemical, and it will volatilize into gas when it exceeds 36°C, which is prone to explosion and production accidents
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[0019] The synthetic production process of this finished product is illustrated as follows:
[0020] first step:
[0021] 200 kilograms of 5-chlorovaleronitrile and 210 kilograms of cyclohexanols are dropped into the first reactor of 500 liters, and 50 kilograms of concentrated sulfuric acid of 98% concentration are dropped into the first reactor, and the temperature is raised to 60 DEG C from room temperature, and the reaction is kept for 15 After the reaction was completed, the temperature was cooled to room temperature for 1 hour to obtain a 5-chloro-N-cyclohexylpentanamide reaction solution. Add 500 kg of water in advance to the 1000 liter second reaction kettle, ice brine in the jacket, and cool the second reaction kettle to 0°C.
[0022] Slowly pump the cooled 5-chloro-N-cyclohexylpentanamide reaction solution in the 500-liter first reaction kettle into the above-mentioned 1000-liter second reaction kettle under a negative pressure of 500-600 mm Hg, and draw the materia...
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Abstract
The invention relates to compounding technology for 5-(4-chlorin butyl)-1-cyclohexyl-1, 2, 3, 4-tetrazole. It adopts 5-chlorin butyl cyanide and cyclohexanol to take reaction to form 5-Cl-N-cyclohexyl pentanamide, adds a little phosphoric chloride, sodium azide into benzene solvent to react to form sample. 5-chlorin butyl cyanide and cyclohexanol are reacting in concentrated sulphuric acid, heating to 60 degree centigrade, keeping for 15 hours, cooling to room temperature, sucking the 5-Cl-N-cyclohexyl pentanamide reaction solution into 0 degree centigrade second reacting kettle, keeping 10 degree centigrade for 4 hours, adding petroleum ether to extract, cooling the organic phase at the third cooling kettle to gain 5-Cl-N-cyclohexyl pentanamide crystal that would be sucked into the fourth reacting kettle, adding toluene solvent adding phosphoric chloride at 0 degree centigrade and heating to 60 degree centigrade for reacting for 2 hours, heating to 112 degree centigrade and keeping for 4 hours, cooling to 25 degree centigrade, being sucked into the fifth reacting kattle, adjusting the pH value to 7 by sodium bicarbonate solution, steaming up toluene at the sixth distiller, adding ethane and cooling to 5 degree centigrade, taking centrifugal separation to the white crystal, drying, the product 5-(4-chlorin butyl)-1-cyclohexyl-1, 2, 3, 4-tetrazole would be gained. The advantage of the invention is that its raw material is low cost, and accidents would be declined.
Description
Technical field: [0001] This product of the 5-(4-chlorobutyl)-1-cyclohexyl-1,2,3,4-tetrazole synthesis production process of the present invention belongs to the intermediate of the synthetic drug cilostazol, and the production process of this product It belongs to the field of a new production process route. Background technique: [0002] 5-(4-Chlorobutyl)-1-cyclohexyl-1,2,3,4-tetrazole products are as follows: the reaction of valerolactone and cyclohexylamine in petroleum ether generates (A) , and then generate product (B) by (A) reacting with phosphorus pentachloride and hydrogen azide in benzene. [0003] [0004] [0005] There are following disadvantages in this traditional reaction route: [0006] 1. The raw material valerolactone needs to be imported, and the price is too high. [0007] 2, the amount of phosphorus pentachloride required in the reaction process from (A) to (B) is relatively large, and the hydrogen chloride discharged easily causes pollution. ...
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