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以1,4-丁二醇、多聚甲醛和干燥的氯化氢气体为原料,合成了氯甲基化试剂1,4-二氯甲氧基丁烷(BCMB),并对白球进行氯甲基化。并采用红外光谱对它们的结构进行了表征。研究了物料配比,溶剂用量,反应温度及反应时间对标题化合物收率的影响。通过正交实验得优化工艺条件为n(1,4-丁二醇)∶n(多聚甲醛)=1∶2,溶剂40 mL,温度6～10℃,反应时间9 h。此条件下,标题化合物收率达到86.73%。
The chloromethylation reagent 1, 4-dichloromethoxybutane (BCMB) was synthesized from 1,4-butanediol, paraformaldehyde and dry hydrogen chloride gas and chloromethylated . Their structures were characterized by infrared spectroscopy. The effects of material ratio, solvent amount, reaction temperature and reaction time on the yield of the title compound were studied. Through orthogonal experiment, the optimal conditions were n (1,4-butanediol): n (paraformaldehyde) = 1: 2, solvent 40 mL, temperature 6 ~ 10 ℃ and reaction time 9 h. Under these conditions, the yield of the title compound reached 86.73%.