Adding a certain compound to certain chemical reactions, such as: 33994-44-4, name is Methyl 3-(4-Iodophenyl)propanoate, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 33994-44-4, name: Methyl 3-(4-Iodophenyl)propanoate
A 500 ml three-neck flask is charged with 14.0 g of 4-(2-thienyl)acetoanilide, 22.4 g of methyl 4-iodophenylpropionate, 13.4 g of potassium carbonate, 0.8 g of copper sulfate pentahydrate and 40 ml of o-dichlorobenzene, and the mixture is stirred under heating at 200 C. for 15 hours in a nitrogen stream. After this reaction, 100 ml of ethylene glycol and 5.4 g of potassium hydroxide are added to the reaction mixture, which is then refluxed under heating for 3 hours in a nitrogen stream, then cooled to ambient temperature, poured into 300 ml of distilled water and neutralized by hydrochloric acid to thereby precipitate crystals. The crystals are filtered, sufficiently washed with water and then transferred to a 1 L flask. To the crystals is added 500 ml of toluene, followed by refluxing under heating to remove water by azeotropic distillation. Then, 100 ml of methanol and 1 ml of concentrated sulfuric acid are added thereto, and the resulting mixture is refluxed under heating for 2 hours in a nitrogen stream. After the reaction, the reaction solution is dissolved in distilled water and extracted with toluene. The organic phase is sufficiently washed with distilled water. Next, the organic phase is dried by sodium sulfate anhydride, a solvent is evaporated off under reduced pressure and the residue is recrystallized from an ethyl acetate-hexane mixed solution to thereby obtain 15.1 g of diarylamine. A 100 ml flask is charged with 5.5 g of the thus-obtained diarylamine, 3.2 g of 4,4-diiodobiphenyl, 2.2 g of potassium carbonate, 0.2 g of copper sulfate pentahydrate and 10 ml of o-dichlorobenzene, and the mixture is refluxed under heating for 9.5 hours in a nitrogen stream. After the reaction is completed, the reaction mixture is cooled to ambient temperature and dissolved in 100 ml of toluene, and unnecessary substances are removed by filtration. An obtained filtrate is purified by silica gel column chromatography using toluene, to thereby yield 6.2 g of a thiophene-containing compound (Exemplary Compound 7). A melting point of the resulting thiophene-containing compound is 110 to 112 C. The IR spectrum (obtained using a KBr tablet method) of the thiophene-containing compound is shown in FIG. 2. An 1H-NMR spectrum (in a CDCl3 solvent) of the thiophene-containing compound is shown in FIG. 3.
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