| 3-氯-6-羟基-2-(甲氧基甲氧基)苯甲醛的合成与表征 |
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| 引用本文： | 仝红娟,刘斌,张翠亚,杜漠.3-氯-6-羟基-2-(甲氧基甲氧基)苯甲醛的合成与表征[J].化学世界,2021,62(2):88-93. |
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| 作者姓名： | 仝红娟 刘斌 张翠亚 杜漠 |
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| 作者单位： | 陕西国际商贸学院医药学院陕西省中药绿色制造技术协同创新中心,陕西西安712046;陕西国际商贸学院医药学院陕西省中药绿色制造技术协同创新中心,陕西西安712046;陕西国际商贸学院医药学院陕西省中药绿色制造技术协同创新中心,陕西西安712046;陕西国际商贸学院医药学院陕西省中药绿色制造技术协同创新中心,陕西西安712046 |
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| 基金项目： | 陕西省自然科学基础研究计划(No.2019JQ-924);陕西省教育厅2018年度专项科学研究计划(No.18JK0954);陕西省大学生创新创业(No.S201913123004)资助项目。 |
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| 摘 要： | 以2,6-二羟基苯甲醛为原料,通过氯代、醚化两步反应,合成得到3-氯-6-羟基-2-(甲氧基甲氧基)苯甲醛.通过对反应条件优化,确定最佳氯代条件为:n(NCS)∶ n(2,6-二羟基苯甲醛)= 1.2 ∶ 1;甲醇为反应溶剂;反应温度50 ℃;反应时间16 h条件下,氯代产物收率达到94.8％.最佳醚化条件为:氢化钠用...
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| 关 键 词： | 苯并呋喃-2-甲酸衍生物 氯代反应 羟基保护 合成 结构表征 |
Synthesis and Characterization of 3-Chloro-6-hydroxy-2-(methoxymethoxy)benzaldehyde |
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| Tong Hongjuan,Liu Bin,Zhang Cuiya,Du Mo.Synthesis and Characterization of 3-Chloro-6-hydroxy-2-(methoxymethoxy)benzaldehyde[J].Chemical World,2021,62(2):88-93. |
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| Authors: | Tong Hongjuan Liu Bin Zhang Cuiya Du Mo |
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| Affiliation: | (School of Pharmacy,Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,Shaanxi Institute of International Trade Commerce,Xi’an,Shaanxi 712046,China) |
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| Abstract: | 3-Chloro-6-hydroxy-2-(methoxymethoxy)benzaldehyde was synthesized from 2,6-dihydr-oxybenzaldehyde through a two-step reaction, involving chlorination and etherification. The reaction conditions were also investigated and the optimal conditions of chlorination were as follows: n(NCS)∶n(2,6-dihydroxybenzaldehyde)=1.2∶1, methanol as solvent at 50 ℃ for 16 h so that the chlorinated product was obtained in a yield of 94.8%. The optimal conditions of etherification were as follows: the dosage of sodium hydride is n(NaH)∶n(3-chloro-2,6-dihydroxybenzaldehyde)=1.5∶1, n(Chloromethyl ether)∶n(3-chloro-2,6-dihydroxybenzaldehyde)=1.4∶1, the reaction was stirred at room temperature for 1 h. 3-Chloro-6-hydroxy-2-(methoxymethoxy)benzaldehyde was then obtained in a yield of 39.3%. The structure of the product and intermediate were identified by 1H NMR and ESI-MS. The structure of the target compound was also confirmed by 1H-1H NOESY. |
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| Keywords: | benzofuran-2-carboxylic acid derivatives chlorination hydroxyl group protection synthesis structure characterization |
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