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化学专业文件翻译  

2013-08-19 10:03:52|  分类: 默认分类 |  标签: |举报 |字号 订阅

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SYNTHESIS: To a 300 mL three-neck round-bottom flask set up with a magnetic stirrer and protected with a N2 atmosphere, there was added 75 mL hexane, 3.5 g tetramethylethylenediamine, and 4.2 g p-dimethoxybenzene.  The reaction mixture was cooled to 0 deg C with an external ice bath, and there was then added 19 mL of 1.6 M butyllithium in hexane.  With stirring, the reaction was brought up to room temperature, and there were produced loose, creamy solids.  There was then added, as a solid and portionwise, 6.6 g diphenyldisulfide which resulted in an exothermic reaction and the production of a nearly clear solution.  After stirring an additional 10 min, the reaction was quenched in 500 mL of dilute NaOH.  The hexane phase was separated, and the aqueous phase extracted with 4x100 mL CH2Cl2 The organic extracts were combined, washed with dilute HCl and the solvents were removed under vacuum to provide 6.0 g of 2,5-dimethoxyphenyl phenyl sulfide as an impure amber oil.  A small sample was saved for microanalysis and NMR, and the re-mainder converted to the corresponding benzaldehyde.

 

A mixture of 6.1 g POCl3 and 5.4 g N-methylformanilide was heated for 3 min on the steam bath, and then added to the remainder of the above-described 2,5-dimethoxyphenyl phenyl sulfide.  The reaction became immediately a deep red and, after heating on the steam bath for 0.5 h, was dumped into a large quantity of H2O, producing a granular brown solid.  This was removed by filtration, and washed sparingly with cold MeOH (the washes were saved).  The resulting pale yellow solids were recrystallized from 20 mL boiling absolute EtOH providing, after cooling, filtration and air drying, 4.4 g of extremely pale yellow crystals of 2,5-dimethoxy-4-(phenylthio)benzaldehyde.  This had a mp of 119-119.5 deg C.  All washes and mother liquors were combined, flooded with H2O and extracted with CH2Cl2.  This solvent was removed under vacuum, and the residue (a viscous oil) was dissolved in a little EtOH which, on cooling in dry ice, gave 1.2 g of a second crop of the aldehyde, mp 117-119 deg C.  Recrystallization from 5 mL 95% EtOH gave an additional 0.4 g product with a mp of 118-119 deg C.  This mp was not improved by recry-stallization from cyclohexane.  The NMR specrum was excellent, with OCH3 singlets (3H) at 3.45 and 3.80 ppm; ArH singlets at 6.28 and 7.26 ppm, the C6H5 as a broad peak centered at 7.50, and the CHO proton at 10.37 ppm.

 

A solution of 4.4 g 2,5-dimethoxy-4-(phenylthio)benzaldehyde in 32 mL nitroethane was treated with 0.8 g anhydrous ammonium acetate and heated on the steam bath for 21 h.  The excess solvent/reagent was removed under vacuum, leaving a dark red oil as residue.  After much diddling and fiddling around, this set up as a crystalline mass. These solids were ground under 20 mL cold MeOH and filtered, providing 5.3 g of the crude nitrostyrene as an orange crystalline residue product after air-drying.  This was ground up under 10 mL MeOH, the insolubles collected by filtration, washed with a little MeOH, and air dried to provide 5.3 g crude 1-(2,5-dimethoxy-4-phenylthiophenyl)-2-nitropropene as yellow crystals, with a mp of 100-102 deg C (with prior sintering at about 98 deg C).  This was recrystallized from 50 mL boiling 95% EtOH.  After cooling in an ice bath, it was filtered, washed with EtOH, and air drying provided gold-yellow crystals with a mp of 105-106 deg C.  The proton NMR was excellent (in CDCl3).


现在想来,这个文件还真够专业的。当时有200多篇,真是一项大工程呀

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