SYNTHESIS OF SPECTROSCOPICALLY PURE DEUTERATED TOLUENE C$sub 6$$H$$sub 5$CD$sub 3$

Journal Article · Mon May 25 00:00:00 EDT 1959 · Compt. rend.

OSTI ID:4242509

Valade, J; Calas, R; Fuson, N; Josien, M

Spectroscopically pure C/sub 6/H/sub 5/CD/sub 3/ was synthesized from phenyllithium and CD/sub 3/Br. The preparation of CD/sub 3/Br is briefly described. The phenyllithium is transferred under an atmosphcre of dry nitrogen to an autoclave cooled to -80 deg C. The CD/sub 3/Br is rapldly added, and the autoclave is brought slowly to room temperature, with agitation. It is then maintained at 100 deg C for 10 hr and cooled. The contents are hydrolyzed and extracted with ether. A first distillation leads to C/sub 6/H/sub 5/CD/sub 3/ contaminated with benzene from the hydrolysis of excess phenyllithium. Two new fractionations are made with a column containing 40 theoretical plates. The compound obtained boils at 108 deg C under normal pressure, corresponding to C/ sub 6/H/sub 5/CD/sub 3/ of at least 99.5% purity. The infrared spectrum is given. (J.S.R.)

• Research Organization: Centre de Physicochimie structurale, Faculte des Sciences, Bordeaux
• NSA Number: NSA-13-015079
• OSTI ID: 4242509
• Journal Information: Compt. rend., Vol. Vol: 248; Other Information: Orig. Receipt Date: 31-DEC-59
• Country of Publication: Country unknown/Code not available
• Language: French

Related Subjects

CHEMISTRY
ABSORPTION
BOILING
BROMINATED HYDROCARBONS
CHEMICAL REACTIONS
COOLING
DEUTERIUM COMPOUNDS
DISTILLATION
EXTRACTION COLUMNS
FLUID FLOW
GASES
HEATING
IMPURITIES
INFRARED RADIATION
LABELLED COMPOUNDS
LITHIUM COMPOUNDS
LOW TEMPERATURE
METHYL RADICALS
MIXING
NITROGEN
OPERATION
ORGANIC BROMINE COMPOUNDS
ORGANOMETALLICS
PHENYL RADICALS
PREPARATION
PRESSURE
PRESSURE VESSELS
QUANTITY RATIO
REACTION KINETICS
REFINING
SPECTRA
SPECTROSCOPY
TEMPERATURE
TOLUENE
WATER