/sup 18/O isotope shift in /sup 15/N NMR spectroscopy. 2. Synthesis of /sup 15/N, /sup 18/O-labeled hydroxylamine hydrochloride

Journal Article · Wed Mar 12 04:00:00 EST 1986 · Inorg. Chem.; (United States)

DOI:https://doi.org/10.1021/ic00226a032· OSTI ID:5681906

Rajendran, G; Van Etten, R L

Since hydroxylamine can serve as a key intermediate in the synthesis of a variety of compounds, the synthesis of (/sup 15/N, /sup 18/O)-labelled hydroxylamine hydrochloride was undertaken. Published procedures for the synthesis of hydroxylamine resulted in poor yields in some cases and in lower percentage of /sup 18/O in the product than expected in other cases. The compound was synthesized in dry tetrahydrofuran (THF) by treating NaNO/sub 2/ with borane-methyl sulfide. The course of the reaction was examined using /sup 11/B NMR spectroscopy, and the product yield was 74%. The /sup 18/O enrichment was demonstrated by both mass spectrometry and /sup 15/N NMR of the isolated acetoxime. 23 references, 1 figure.

• Research Organization: Purdue Univ., West Lafayette, IN
• OSTI ID: 5681906
• Journal Information: Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 25:6; ISSN INOCA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400302* -- Organic Chemistry-- Isotope Effects-- (-1987)
ALKANES
AMINES
BORON COMPOUNDS
CHEMICAL PREPARATION
EVEN-EVEN NUCLEI
FURANS
HETEROCYCLIC COMPOUNDS
HYDROCARBONS
HYDROXYLAMINE
ISOTOPES
LABELLED COMPOUNDS
LIGHT NUCLEI
NITROGEN 15
NITROGEN ISOTOPES
NUCLEI
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
OXYGEN 18
OXYGEN ISOTOPES
STABLE ISOTOPES
SYNTHESIS
TETRAHYDROFURAN