Green production process of uracil

A technology of green production and uracil, applied in the field of green production technology of uracil, which can solve the problem of increasing the amount of wastewater and achieve the effect that the yield and purity will not be affected

Inactive Publication Date: 2018-06-22
无锡富泽药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Inadequacies of the literature route one: the process can produce 30 tons of sulfuric acid and 50 tons of waste water per ton of uracil product
[0014] The second deficiency of the literature route: Although this process overcomes the generation of a large amount of waste sulfuric acid in the traditional process, the amount of waste water increases to 40 tons of waste water per ton of product

Method used

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  • Green production process of uracil
  • Green production process of uracil
  • Green production process of uracil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 50 grams of thiouracil (3M) to 130 mL of water and 5.0 grams (6 equivalents) of chloroethanol, stir to raise the temperature to 100 degrees, reflux overnight, cool down slightly, analyze crystal uracil, and filter and dry. Yield 95%, purity (HPLC) 99.0%. Mother liquor continues to add 50 gram thiouracils, heats, and cycle above-mentioned operation, mother liquor can be used continuously five times. The average yield is 91%. M.P.>300°C. 1HNMR (CDCl 3 , TMS) (δ, ppm): 8.546 (d, 1H, =CH-N); 7.360 (d, 1H, =CH-C). Purity was not affected (see table below).

[0037] Mother liquor cycle times

Embodiment 2

[0039] Add 50 grams of thiouracil (3M) to 130 mL of water and 5.0 grams (6 equivalents) of bromoethanol, stir to raise the temperature to 100 degrees, reflux overnight, cool down slightly, analyze crystal uracil, and filter and dry. Yield 85%, purity (HPLC) 99.1%. Mother liquor continues to add 50 gram thiouracils, heating, cycle above-mentioned operation, mother liquor can use five times continuously. The average yield is 80%; M.P.>300℃. 1HNMR (CDCl 3 , TMS) (δ, ppm): 8.546 (d, 1H, =CH-N); 7.360 (d, 1H, =CH-C). Purity was not affected (see table below). Purity has little effect.

[0040]

[0041]

Embodiment 3

[0043] Add 50 grams of thiouracil (3M) to 130 mL of water and 5.0 grams (6 equivalents) of chloroacetic acid, stir to raise the temperature to 100 degrees, reflux overnight, cool down slightly, analyze crystal uracil, and filter and dry. Yield 90%, purity (HPLC) 99.0%. Mother liquor continues to add 50 gram thiouracils, heating, cycle above-mentioned operation, mother liquor can use five times continuously. The average yield is 94%; M.P.>300°C. 1HNMR (CDCl 3 , TMS) (δ, ppm): 8.546 (d, 1H, =CH-N); 7.360 (d, 1H, =CH-C). Purity was not affected (see table below). Purity is not affected.

[0044] Mother liquor cycle times

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PUM

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Abstract

The invention provides a green production process of uracil. The process comprises the following steps that (1) thiouracil is used as raw materials; water is added; a halogenide or a sulfur acid compound is also added; heating for the night, temperature reduction and filtering drying are performed to obtain high-purity uracil; (2) the thiouracil is continuously added into mother liquid obtained through filtering in the step (1); heating is performed; the operations are cycled. The green production process has the following technical effects that the reaction mother liquid and the materials canbe used indiscriminately; the yield and the purity are not influenced; the process belongs to a green and environment-friendly process. The high-purity uracil can be obtained; the HPLC detection purity is 95 percent or higher; even the uracil being 98 percent or higher can be obtained.

Description

technical field [0001] The invention relates to a green production process of uracil, which belongs to the technical field of chemical industry. Background technique [0002] Uracil is the stable ketone structure of 2,4-dihydroxypyrimidine. It is an intermediate in the synthesis of antineoplastic drug 5-fluorouracil and its derivatives, such as tegafur, bisfurfururacil, doxifluridine, carmofur and antiviral 5-iodo-2'-deoxyuridine. [0003] Synthetic route has following several in the prior art: [0004] Literature route one: [0005] [0006] Process: Add 70mL oleum to a 200mL clean reaction bottle, turn on the ice machine to lower it to 0°C, add 25g of urea while stirring, and control the process temperature below 10°C. Add 50g of malic acid, heat up to 90°C, stir for 3h, and adjust the pH to 6 with sodium hydroxide solution. After suction filtration, 70g of light red crude product was obtained. The crude product was recrystallized with 350ml of water to obtain 50g ...

Claims

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Application Information

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IPC IPC(8): C07D239/54
CPCC07D239/54
Inventor 吴鹏程李浩源谢卫锋孔献
Owner 无锡富泽药业有限公司
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