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Chapter – 2 Microwave assisted simple and fast…..
2.4 EXPERIMENTAL
2.4.1 PREPARATION OF 2 – METHYL INDOLINE
It was prepared according to method described in Chapter – 1.
2.4.2 GENERAL PROCEDURE FOR THE PREPARATION OF DNJ-301 TO
DNJ-305
STEP – 1 GENERAL PROCEDURE FOR THE PREPARATION OF SIDE
CHAINS SC-01 TO SC-05
It was prepared according to the method described by Liu et. al. a To a
stirred solution of 0.127 mole of 1-bromo-3-chloro propane in 100 ml toluene,
0.28 mole of an appropriate secondary amine was added at 75°C. The
reaction mixture was stirred at this temperature for 4 hours. The progress and
the completion of the reaction were checked by silica gel-G F254 thin layer
chromatography using dichloromethane : methanol (20 : 1) as mobile phase.
After the reaction to be completed, it was filtered to remove the precipitation,
and the filtrate was concentrated under vacuum to afford crude liquid which
was used as such without further purification as the material was pure enough
for the subsequent reactions.
Code
No.
Substitution
R1 & R2
% Yield
SC-01 Piperidine 66
SC-02 Morpholine 70
SC-03 1-Methyl Piperazine 62
SC-04 1-Ethyl Piperazine 64
SC-05 1-Benzyl Piperazine 60
STEP – 2 GENERAL PROCEDURE FOR THE PREPARATION OF DNJ-
301 TO DNJ-305
a H. Liu, L. Smith, Y. Mao, W. Pan, Y.-J. Xu, S. Burdzovic-Wizeman, M. Duneton and W.
Wong; Synth. Commun., 2006, 36 (3), 347.
Department of Chemistry, Saurashtra University, Rajkot – 360 005 79