Compound with intramolecule change transfer and its preparing process
A technology for charge transfer and compounds, applied in the field of compounds with intramolecular charge transfer and their preparation
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[0017] The preparation method of the compound described in the present invention is described further below: (1) 2-(4,5-di-n-hexylthio-1,3-dithio-2-ylidene)-5-hydroxymethylene-5 - Preparation of hydrogen-6-dihydro-1,3-dithio[4,5-b][1,4]dithiocyclohexane:
[0018] After Zincate is dissolved in acetone, add hexyl bromide dissolved in acetone dropwise in boiling state, wherein the molar ratio of Zincate and hexyl bromide is 1:5.3, continue to reflux for 2-4 hours, and remove insoluble matter by suction filtration. The solvent was distilled off, and the residue was purified by column chromatography to obtain 4,5-di-n-hexylthio-1,3-dithiol-2-thione, one of the raw materials required for the coupling reaction. The reaction formula is as follows: Show:
[0019] After reflux for 20 hours in the same way, another raw material 5,6-dihydro-5-acetoxymethylene-1,3-dithio[4,5-b][1,4] was purified to obtain the coupling reaction Dithiocyclohexane-2-thione.
[0020] In order to improve...
Embodiment 4
[0026] Example 4, 5-di-n-hexylthio-1,3-dithiole-2-thione
[0027] 8g Zincate (11.2mmol) was dissolved in 100mL acetone, heated to reflux with stirring, 50mL acetone solution containing 9.4mL (60mmol) bromohexane was added dropwise, and refluxed for 4 hours. Suction filtration to remove insoluble matter. Acetone was removed by rotary evaporation. The residue was subjected to column chromatography (chloroform:petroleum ether=1:2 as the developing solvent) and the developing solvent was rotated to obtain 8 g of orange-red oil with a yield of 98%. MS(EI): m / z(%)=367(M + +1, 14.119), 366 (M + , 27.196) 5,6-dihydro-5-acetoxymethylene-1,3-dithio[4,5-b][1,4]dithiocyclohexane-2-thione
[0028] Add 7.2g (10mmol) Zincate and 100mL acetone into a 250mL three-neck flask. 11.4 mL (80 mmol) 2,3-dibromopropyl acetate / 50 mL acetone were added dropwise under stirring and reflux, and the reaction was carried out for about 20 hours. TLC tracking, the developing solvent...
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