2003年西北大學(xué)化學(xué)系有機(jī)化學(xué)碩士研究生復(fù)試題(共3頁,17道題,滿分100分,可以不抄題,寫清題號(hào)
1. 請(qǐng)敘述你參加過或正在從事的科研課題的題目、意義、成果,并隨卷子寄來你發(fā)表的論文、學(xué)士論文。若應(yīng)屆生尚未完成學(xué)士論文的,請(qǐng)你的指導(dǎo)教師在你寫的本題答案后簽字。(10分)
2. 有機(jī)化合物結(jié)構(gòu)測(cè)定前為什么要先做樣品的純度檢驗(yàn)?請(qǐng)敘述有機(jī)化合物的純度檢驗(yàn)如何進(jìn)行?(5分)
3. 下列兩個(gè)化合物中Ha和Hb的化學(xué)位移哪個(gè)大?為什么?(2分)
4. 有一個(gè)化合物的分子量為116,MS中M :M+1峰豐度比為100:6.5,在C6H14NO ;C6H12O2 ;C8H4O三個(gè)式子中哪個(gè)是可能的分子式?說明理由。(4分)5.在常溫下,下列有*號(hào)的質(zhì)子在1H-NMR中出幾重峰(CDCl3溶劑)(4分)
6.某化合物的質(zhì)譜部分?jǐn)?shù)據(jù)如下,推測(cè)可能的分子式,寫出推測(cè)過程:(5分) m/z 104 105 121 122 123 124 RI 13 1.0 89 100 7.9 0.7 7.某種農(nóng)藥的合成步驟如下:(5分) 產(chǎn)物的 1HNMR數(shù)據(jù)如下: δ1.34(d,6H); δ4.32(s,2H); δ5.8(m,1H); δ7~7.8(m,5H)請(qǐng)推測(cè)產(chǎn)物的結(jié)構(gòu),寫出推測(cè)過程。
8.有一化合物分子式C7H6O,其IR光譜圖如下,試推測(cè)結(jié)構(gòu),寫出推測(cè)過程。 (5分)
9. 將以下段落翻譯為中文(5分)The importance of carbanions in synthesis is exemplified by the Grignard and Wittig reactions. Although they are among the most versatile and useful reactions in organic chemistry, carbanion-based reactions are generally known to be very sensitive towards air and water. The required deviation from ambient conditions along with the commonly used methods for their generation leads to several fundamental drawbacks when the Principles of Green Chemistry are applied: (1) large volumes of anhydrous organic solvents are required which could potentially increase volatile organic emissions; (2) anhydrous conditions require excess drying agents which leads to unwanted waste; (3) anhydrous conditions also require the protection of functional groups such as hydroxy groups and carboxylic acids; (4) the requirement of inert gas atmosphere implies that the catalyst is prone to deactivation, which will increase the amounts of metal waste; (5) requirement of stoichiometric amounts of metals also leads to a large amount of metal waste; and (6) the general use of organic halides as the carbanion source will generate a stoichiometric amount of halide waste, as well as requiring multi-step synthesis of halides.
10. 減壓蒸餾裝置中導(dǎo)氣毛細(xì)管有什么作用? 如不用導(dǎo)氣毛細(xì)管, 用什么方法可以代替?該替代辦法除起到毛細(xì)管的作用外,還有什么優(yōu)點(diǎn)? (5分)
11. AlCl3催化苯與醋酸酐反應(yīng)制備苯乙酮實(shí)驗(yàn)中, 隨著醋酸酐的逐漸加入反應(yīng)瓶?jī)?nèi)會(huì)有什么現(xiàn)象變化? (3分)
12. 在萃取中, 有哪些方法可以用來判斷有機(jī)層是在上層或下層? (3分)13. 水蒸氣蒸餾如何判斷蒸餾結(jié)束? (3分)
14. 一般從庫房中領(lǐng)到的苯甲醛其瓶中有少量白色固體,此白色固體是什么?(3分)
15. 薄層色譜中,樣品Rf數(shù)值如果太大或太小,如何調(diào)節(jié)?(4分)
16. 有機(jī)溶劑重結(jié)晶應(yīng)采用什么樣熱溶解裝置?對(duì)于冷卻后容易析出的化合物在熱過濾時(shí)如何避免損失?(4分)
17. 由指定原料合成目標(biāo)物,其它試劑自選 (30分)
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