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qinchangming

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专业: 金属有机化学

[求助] 急问关于一个合成的问题,非常感谢!

大家好,我最近合成一个化合物,碰到了问题,请教大家,非常感谢!

文献的方法是:
Inorg. Chem. 2003, 42, 2977-2982

Synthesis of L3. Diisoproylamine (3.8 mL, 27 mmol) and
n-BuLi (11.4 mL, 2.5 M in hexane) were dissolved in a 60 mL of
THF in a Schlenk flask at -78 °C. After the solution was stirred
for 30 min at -78 °C, 2-picoline (2.5 mL, 25 mmol) was added to
the solution. The solution was allowed to warm to room temperature
and stirred for 30 min. To the solution was added p-tolualdehyde
(1.0 mL, 8.4 mmol). The resulting solution was stirred overnight
and quenched with water (100 mL). After the reaction mixture was
washed with saturated NaHCO3 (100 mL), CH2Cl2 (100 mL) was
added to extract the dipyridyl compound. The CH2Cl2 layer was
dried over anhydrous MgSO4, concentrated, and chromatographed
on a silica gel column eluting with hexane and diethyl ether (v/v,
1:1). Removal of the solvent gave the product in 36% yield

A similar reaction involving formyl acetate afforded a tripodal ligand of L2

我的目标是合成L2.

首先我第一步用Diisoproylamine和n-BuLi 合成LDA时,碰到了个问题, 我非常注意无水无氧了,但是合成出来的是蓝绿色的THF溶液,很奇怪.

其次,我完全按照文献上的操作,但是没有一点目标产物,而是合成出来了一个新的化合物 (我重复了结次,都是这样的结果).

我检查不出我是哪个地方出了问题,我感觉我做的很仔细了啊, 但是老板说文献不可能错了, 而且文献的思路是正确的啊,我想也是,但怎么就是做不出来呢?

请教以下各位大侠, 非常感谢!

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