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北京石油化工学院2026年研究生招生接收调剂公告
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whb265

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[求助] 求助Boc亚胺的合成方法

求助Boc亚胺的合成方法

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whb265

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N上无氢,编辑错误
2楼2010-10-26 18:42:01
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121918051

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YUE-jf(金币+1):积极回帖奖励 2010-10-27 11:18:42
whb265(金币+1, 博学EPI+1): 2010-10-28 17:32:04
用苯甲醛和Boc胺在碱性条件下就可以得到,反应很容易,加氢氧化钠研磨就可以,醛和胺的摩尔比为1:1。
3楼2010-10-27 09:29:56
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121918051

至尊木虫 (著名写手)

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氢氧化钠为4摩尔
4楼2010-10-27 12:47:45
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whb265

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有相关文献吗
5楼2010-10-29 09:28:39
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寒月龙飞

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两步做:先合成氨基亚砜类化合物,第二部用碳酸钾催化脱去亚磺酸集团。一 A 500-mL flask was charged
with tert-butyl carbamate (10.0 g, 85.5 mmol, 1.00 equiv) and
benzenesulfinic acid sodium salt (28 g, 170 mmol, 2.0 equiv). Solids were
suspended in a solution of methanol in water (1:2, 250 mL). Benzaldehyde
(13.0 mL, 128 mmol, 1.50 equiv) was then added in one portion, followed by
formic acid (98%, 6.4 mL). The reaction was allowed to stir 48 h at 23 °C,
during which time the product precipitated as a white solid. which was isolated via Büchner funnel
filtration and purified via trituration with water and diethyl ether. After drying in vacuo, 7a was
obtained as a white solid (23.6 g, 80%).二 A 250-mL, 3-neck flask was charged with
anhydrous potassium carbonate (12.4 g, 90.0 mmol, 6.00 equiv) and anhydrous
sodium sulfate (15 g). The solids were placed under vacuum and flame-dried.
Once cool, 7a (5.2 g, 15 mmol, 1.0 equiv) was added under a positive stream of
nitrogen, followed by anhydrous tetrahydrofuran (140 mL). The flask was
capped with a water-cooled reflux condenser under an atmosphere of nitrogen
and heated to reflux with stirring. After 15 h, the reaction was cooled to ambient temperature and
the solids removed via filtration through a fine, glass frit. The filtrate was concentrated in vacuo
and dried under high vacuum to give imine  as a colorless oil
6楼2010-11-08 20:24:51
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寒月龙飞

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whb265(金币+10): 2010-11-13 12:01:01
J. Am. Chem. Soc., 2002, 124 (44), pp 12964–12965
参考文献
7楼2010-11-08 20:26:23
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寒月龙飞

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费劲给你查的 呵呵 !
8楼2010-11-08 20:28:11
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