Direct observation of the unstable intermediates in radical addition reaction by using an interfacing microchip combined with an NMR

被引：12

作者：

Nakakoshi, Masamichi ^{[1
]}

Ueda, Masafumi ^{[2
]}

Sakurai, Satoshi ^{[3
]}

Asakura, K. ^{[3
]}

Utsumi, Hiroshi ^{[3
]}

Miyata, Okiko ^{[2
]}

Naito, Takeaki ^{[2
]}

Takahashi, Yutaka ^{[3
]}

机构：

[1] Yokohama Natl Univ, Ctr Chem Anal, Hodogaya Ku, Yokohama, Japan

[2] Kobe Pharmaceut Univ, Kobe, Hyogo 6588558, Japan

[3] JEOL Ltd, Tokyo 1968558, Japan

来源：

MAGNETIC RESONANCE IN CHEMISTRY | 2007年 / 45卷 / 11期

关键词：

nuclear magnetic resonance; micro channeled cell for synthesis monitoring; B-11; intermediate; oxime ether; Et3B; radical reaction;

D O I：

10.1002/mrc.2087

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

Direct observation of the unstable intermediate in the radical addition reaction of the oxime ether 1 mediated by triethylborane (Et3B) is described using H-1 and B-11 micro channeled cell for synthesis monitoring (MICCS), which was recently developed as an interfacing microchip for NMR. It was possible that the signal of the intermediate was observed as a result of using MICCS technique with a standard NMR instrument. This result supports the structure of the intermediate analyzed by diffusion-ordered spectroscopy (DOSY) NMR method in a previous paper. The procedure of micro channeled cell for synthesis monitoring-nuclear magnetic resonance (MICCS-NMR) was much easier than that of DOSY method. It was proven that it could be applied to the reaction in an anhydrous condition. Copyright (c) 2007 John Wiley & Sons, Ltd.

引用

页码：989 / 992

页数：4

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