Synthesis of 2,4-dichloro-5-fluoropyrimidine and recovery of DMA from waste water

FU Yongfeng; GUO Ning; YUN Zhi; SUN Shanshan

doi:10.11949/j.issn.0438-1157.20141261

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Synthesis of 2,4-dichloro-5-fluoropyrimidine and recovery of DMA from waste water

更新时间：2025-12-10

- Synthesis of 2,4-dichloro-5-fluoropyrimidine and recovery of DMA from waste water
- CIESC Journal Issue 5, Pages: 1723-1729(2015)
- 作者机构：
  
  1. 南京工业大学化学化工学院,江苏,南京,210009
  2. 齐鲁工业大学化学与制药工程学院,山东,济南,250353
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20141261
  CLC： Q254.1
- Online First：05 May 2015，
  
  Published：05 May 2015
- 稿件说明：
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FU Yongfeng, GUO Ning, YUN Zhi, et al. Synthesis of 2,4-dichloro-5-fluoropyrimidine and recovery of DMA from waste water[J]. CIESC Journal, 2015, (5): 1723-1729.
DOI：

FU Yongfeng, GUO Ning, YUN Zhi, et al. Synthesis of 2,4-dichloro-5-fluoropyrimidine and recovery of DMA from waste water[J]. CIESC Journal, 2015, (5): 1723-1729. DOI： 10.11949/j.issn.0438-1157.20141261.

摘要

使用5-氟尿嘧啶(5-FU)和三氯氧磷(POCl3)作为原料、N

N-二甲基苯胺(DMA)作为缚酸剂合成2

4-二氯-5-氟嘧啶

系统研究了5-FU与POCl3的摩尔比、5-FU与DMA的摩尔比、反应温度和反应时间对反应收率的影响

简要阐述该反应机理。反应结束后

向废液中加入NaOH固体对废液进行处理

探讨DMA的回收率和副产物磷酸氢二钠的收率与pH的关系。结果表明

在工艺参数为5-FU与POCl3的摩尔比为1:10、5-FU与DMA的摩尔比为1:1.5、回流温度114℃、回流时间2 h时

4-二氯-5-氟嘧啶的收率为92.2%;通过加入NaOH固体将废液pH调至7

DMA的回收率和副产物磷酸氢二钠的收率都为最大值。

Abstract

4-Dichloro-5-fluoropyrimidine was prepared by reaction of 5-fluorouracil (5-FU) and phosphorus oxychloride in the presence of N

N-dimethylaniline (DMA) as acid acceptor. The effect of molar ratio of 5-FU to phosphorus oxychloride

molar ratio of 5-FU to N

N-dimethylaniline

reaction temperature and reaction time was investigated. Furthermore

reaction mechanism was discussed. 5-FU and POCl3 ratio 1:10

5-FU and DMA ratio 1:1.5

reaction temperature 114℃

reaction time 2 h were the optimum process parameters of synthesizing 2

4-dichloro-5-fluoropyrimidine. Under this process condition

maximum yield of 92.2% of 2

4-dichloro-5-fluoropyrimidine could be obtained. The pH of waste water was then adjusted by adding sodium hydroxide

and the effect of pH on recovery of DMA and yield of by-product disodium hydrogen phosphate was studied. When pH was adjusted to 7

maximum recovery of DMA and maximum yield of by-product disodium hydrogen phosphate could be obtained.

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