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The product synthesized under the optimum conditions as follows had final acid value of 0.494 mgKOH/g,and conversion of reatants up to 99.59%,molar ratio of isooctanol to phthalic anhydride 3∶1,the dosage of both aluminium oxide and stannous octoate as catalyst 0.2%(based on the total mass of reactants),reaction time 2.5 hours.

考察了工艺条件对合成DOP的影响,结果表明,在异辛醇与苯酐摩尔比3∶1,氧化铝/辛酸亚锡复配催化剂用量分别占反应物总量的0.2%,反应温度230℃,反应时间2.5h的最佳工艺条件下,产品终点酸值0.494mgKOH/g,反应物转化率达99.59%。

Methods: 2ethyl aniline was used as starting material of the synthesis and was processed by acetic anhydride acylation, strong nitric acid nitraction at low temperature, and desacyl synthesis to produce 2ethyl5nitro aniline. The product was then synthesized to 3methyl6nitro1Hindazole by using ringclosing reaction in the presence of NaNO2, and then ethylated to obtain 2,3diethyl6 nitro2Hindazole. The latter compound was then reduced by SnCl2/Hcl to get target compound 2,3diethyl6nitro2Hindazole.

以2乙基苯胺为原料经醋酐酰化、浓硝酸低温硝化及去酰基保护合成2乙基5硝基苯胺,后用亚硝酸钠关环得3甲基6硝基1H吲唑,经硫酸二甲酯甲基化得2,3二甲基6硝基2H吲唑,最后用氯化亚锡将其还原得到目标产物,通过1H NMR确定结构与目标产物一致。

Methods: 2-ethyl aniline was used as starting material of the synthesis and was processed by acetic anhydride acylation, strong nitric acid nitraction at low temperature, and desacyl synthesis to produce 2-ethyl-5-nitro aniline. The product was then synthesized to 3-methyl-6-nitro-lH-indazole by using ring-closing reaction in the presence of NaNO2, and then ethylated to obtain 2, 3-diethyl-6- nitro-2H-indazole. The latter compound was then reduced by SnC12/Hcl to get target compound 2, 3-diethyl-6-nitro-2H-indazole.

以2-乙基苯胺为原料经醋酐酰化、浓硝酸低温硝化及去酰基保护合成2-乙基-5-硝基苯胺,后用亚硝酸钠关环得3-甲基-6-硝基-1H-吲唑,经硫酸二甲酯甲基化得2,3-二甲基-6-硝基-2H-吲唑,最后用氯化亚锡将其还原得到目标产物,通过1HNMR确定结构与目标产物一致。

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