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zhangwei章薇鐵蟲 (初入文壇)
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[求助]
幫幫忙,翻譯一下,謝謝。
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Synthetic procedure for the various 4-dialkylaminobenzaldehydes A mixture of aniline (0.26 g, 2.8 mmol), 1-alkylbromide (7.5 mmol), and K2CO3 (1.38 g, 10 mmol) in DMF (20 mL) was stirred for 24 h at 80 ℃ and then cooled to room temperature and poured into water and extracted with ether. After the solvent was removed by a rotatory evaporator, the crude product was dried in vacuo and then added to a stirring solution of phosphoryl trichloride (5 mL) and DMF (20 mL) at room temperature and stirred for 6 h. The resulting mixture was poured into ice-water and extracted with ether. The solvent was evaporated and the crude product was separated by column chromatography on silica gel using hexane–ethyl acetate (15/1) as the eluent. Colourless or a slight yellow oil was obtained in high yields of 80–90%. These compounds were characterized by 1H NMR and the relative data was as follows. |

至尊木蟲 (知名作家)
Translator and Proofreader
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各種4-二烷基氨基苯甲醛的合成過程 苯胺(0.26克,2.8毫摩爾),1 - 烷基溴化物(7.5毫摩爾)和K2CO3(1.38克,10毫摩爾)在DMF(20mL)中的混合物,在80℃攪拌24小時,然后冷卻至室溫,并傾入水中并用用乙醚萃取。用旋轉(zhuǎn)蒸發(fā)器除去溶劑后,將粗制品在真空中干燥,然后加入到磷酰三氯(5毫升)和DMF(20mL)中在室溫下攪拌6小時。將所得混合物傾入冰水中,并用乙醚萃取。蒸發(fā)溶劑后,用硅膠柱層析分離粗制品,用己烷 - 乙酸乙酯(15比1)作洗脫液。在80-90%的高收率處得到無色或淡黃色油。這些化合物用1H進(jìn)行 NMR分析,相對數(shù)據(jù)如下。 |
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