Premium
A facile synthesis of ( 15 N 2 ) malononitrile
Author(s) -
Laxer Avital,
Fischer Bilha
Publication year - 2000
Publication title -
journal of labelled compounds and radiopharmaceuticals
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.432
H-Index - 47
eISSN - 1099-1344
pISSN - 0362-4803
DOI - 10.1002/(sici)1099-1344(200001)43:1<47::aid-jlcr289>3.0.co;2-k
Subject(s) - malononitrile , chemistry , reagent , diethyl malonate , acetonitrile , yield (engineering) , organic chemistry , malonate , combinatorial chemistry , catalysis , materials science , metallurgy
The first synthesis of doubly 15 N‐labelled malononitrile is described and its spectral properties are provided. A highly pure ( 15 N 2 ) malononitrile is obtained in a facile and simple two‐step synthesis which include reaction of diethyl malonate with 25% 15 N 4 OH at room temperature overnight to form ( 15 N 2 )‐malonodiamide in 84% yield, and dehydration of the latter by POCl 3 in acetonitrile to ( 15 N 2 ) malononitrile (75%). The choice of reagents, and simple solutions for work‐up, are discussed. Copyright © 2000 John Wiley & Sons, Ltd.