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Synthesis of 14C-labelled compounds. I. Synthesis of 2 (14C)-dinitrosohexahydropyrimidine

✍ Scribed by Horst Brann; Barbara Bertram; Manfred Wiessler

Publisher
John Wiley and Sons
Year
1977
Tongue
French
Weight
184 KB
Volume
13
Category
Article
ISSN
0022-2135

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✦ Synopsis

Abstract

A convenient procedure to synthesize 2–^14^C‐dinitroso‐hexahydropyrimidine (DNHP) is described. The synthesis begines with the condensation of ^14^C‐formaldehyde and propylenediamine‐1,3 in benzene with azeotropic removal of water. The resulting bases are isolated from the reaction mixture as hydrochlorides and are nitrosated with sodium nitrite in aqueous medium at a constant pH of 4 to 5. After column chromatography on Silica gel and recrystallisation from ether 2–^14^C‐dinitroso‐hexahydropyrimidine (DNHP) is isolated in 30.7% yield based on ^14^C‐fomaldehyde.

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