"Synthesis of (3,4-methylenedioxyphenyl)-2-propanone."
Xiao, Guo-min; Gu, Hai-ming; Zhang, Jin (Department of Chemistry
and Chemical Engineering, Southeast University, Nanjing 210096,
Peop. Rep. China). Jingxi Huagong, 18(6), 321-324 (Chinese) 2001
Jingxi Huagong Bianjibu. CODEN: JIHUFJ. ISSN: 1003-5214.
DOCUMENT TYPE: Journal CA Section: 1 (Pharmacology))
A process for the prepn. of (3,4-methylenedioxyphenyl)-2-propanone
was studied by means of epoxidn. of safrole and subsequent catalytic
isomerization of the so-obtained epoxide.
(3,4-Methylenedioxyphenyl)-2-propanone is a useful intermediate for
the synthesis of methyldopa, an important antihypertensive agent.
The optimal result was obtained by expts. done under various
conditions, such as kind of catalyst, consumption of catalyst and
reaction time. The yield of epoxidn. achieved 92% at
n(catalyst):n(safrole) = 0.0039, n(catalyst):n(H2O2) = 0.0046,
n(H2O2):n(safrole) = 0.87, reaction time 4 h, reaction temp.356-358K
and with 1,2-dichloroethane as solvent. The yield of isomerization
achieved 91% at n(LiI):n(crude product) = 0.045, reaction time 6 h,
reaction temp. 351-353 K, with Et acetate as solvent and LiI as
catalyst. Purity of the title compd. was over 95%.
"Whatever there is to learn has to be learned the hard way."
Castaneda's teacher Don Juan Matus