求助:氨基卟啉和三光氣的反應(yīng)
[font=]有誰做過:5-(4-氨基苯基)-10,15,20-三苯基卟啉和三光氣反應(yīng),生成異氰酸酯卟啉
看到有人這么做的,13 mg(4.16×10-5 mol)三光氣用10 mL 無水1, 2-二氯乙烷溶解后,緩慢滴加到溶于20 mL 無水1, 2-二氯乙烷的70 mg 單氨基卟啉(1.11×10-4 mol)和三乙胺(31 μL;4.68×10-4 mol),上述操作在氮?dú)獗Wo(hù)下進(jìn)行,然后在氮?dú)獗Wo(hù)下,回流攪拌3h
我做了幾次,發(fā)現(xiàn)滴加三光氣后,有一個(gè)新點(diǎn),再加熱,沒有變化,那個(gè)新點(diǎn)測(cè)質(zhì)譜不是,很苦惱,不知錯(cuò)在哪料,希望有人指點(diǎn)
[ Last edited by Pd7577 on 2010-9-12 at 09:39 ]
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Preparation of receptor 5: Triphosgene (13 mg, 4,16 x
10-5 mol) was added to a solution of 1 (70 mg; 1.11 x 10-4
mol) and Et3N (31 μl; 4.68 x 10-4 mol) in anhydrous 1,2-
dichlorethane (20 ml) in atmosphere of N2 and the resulted
mixture was stirred under reflux for 3 h.
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