定制各类格氏试剂

问题:急需,请教一反应!
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提问:kangrui369
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时间:2008-05-24 10:36:12  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

哪位知道用丙二腈和甲酸甲酯(或乙酯)如何制备乙氧基亚甲基丙二腈?


[该帖子已被kangrui369在2008-05-24 10:39:42编辑过]
回复人:afc,★★ (氟化学产品) 时间:2008-05-24 11:06:52   编辑 1楼
下面是用丙二腈和原甲酸三乙酯合成的,共参考!
malononitrile3.3g(50.Ommo1),ethyl orthoformate 11.1g (75.0
mmo1)and acetic anhydride 12.8g(125.5
mmo1)were mixed in a three neeked flask with
stirring.The mixture was refluxed for 6h at
95℃ .Then a little charcoalwas added. The
solvent was removed from the mixture by disti1
lation.The hot residue was filtered and the
filter cake was washed with hot ethano1.the
filtrate was placed in a refrigeretor overnight.
After filtradon, the crystalline Was washed
witl1 ice—cold ethanol and dried to get 3 5.Og,
yield 82.5%,mp:66~C~ 68

[该帖子已被afc在2008-05-24 11:09:21编辑过]


回复人:kangrui369, () 时间:2008-05-24 11:35:36   编辑 2楼
丙二腈和原甲酸三乙酯合成我已经用过了,成本太高。




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