| 崔志华,张淑芬,杨锦宗,汤立军.萘酚磺酸类偶氮化合物酰氯化研究[J].,2008,(1):26-32 |
| 萘酚磺酸类偶氮化合物酰氯化研究 |
| Research on sulfonyl chlorination of sulfonate-containing naphthol azo compounds |
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| DOI：10.7511/dllgxb200801006 |
| 中文关键词: 偶氮化合物 酰氯化反应 酰氯化试剂 溶剂 结构验证 |
| 英文关键词: azo compound reaction of sulfonyl chlorination reagent of sulfonyl chlorination solvent structural identification |
| 基金项目:国家自然科学基金资助项目(20276009). |
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| 中文摘要: |
| 以萘酚磺酸类偶氮化合物酸性橙7为原料，氯化亚砜为酰氯化试剂，N,N-二甲基甲酰胺(DMF)为催化剂，合成重要的染料中间体磺酰氯化合物. 选择不同极性试剂作为酰氯化反应的溶剂，考查了不同溶剂对酰氯化收率和选择性的影响，并探讨了DMF在反应体系中的作用以及酰氯化反应的机理；其中以苯、甲苯和氯化亚砜作溶剂，反应选择性好，收率均高于89%. 此外，鉴于磺酰氯在质谱与核磁分析中的不稳定性，以稳定的磺酰胺分析代替直接的磺酰氯分析，间接地证明了磺酰氯的分子结构. |
| 英文摘要: |
| Chlorosulfonyl-containing naphthol azo compounds were prepared by reaction of the corresponding sodium sulfonate (C.I. Acid Orange 7) with thionyl chloride in the presence of a catalytic quantity of N,N-dimethylformamide and some different solvents. The yield and chemical selectivity of chlorosulfonyl-containing naphthol azo compounds are discussed according to the properties of different solvents. It was demonstrated that high selectivity and high yield(>89%) were achieved by using benzene, toluene or thionyl chloride as solvent. Additionally, on account of unstable properties of sulfonyl chlorides in MS and 1H NMR analyses, a new analytical method using stable sulfonamide is put forward to testify the molecular structures of sulfonyl chlorides indirectly. |
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