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Chapter – 2 Microwave assisted simple and fast…..
0.01 mole of an appropriate side chain (SC-01 to SC-05) was charged
into 250 ml erlenmeyer flask loosely covered with gravity funnel. 0.015 mole
of anhydrous potassium carbonate was added followed by addition of 0.01
mole of 2-methyl indoline into above flask. 1 ml of dimethylformamide was
added in order to make slurry. The reaction mixture was irradiated under
microwave irradiation into household microwave oven (LG MS-192 W) at 480
W for desired time. The progress and the completion of the reaction were
checked by silica gel-G F254 thin layer chromatography using toluene : ethyl
acetate (7 : 3) as mobile phase. The reaction mixture was then taken into 50
ml water and it was extracted with ethyl acetate (30 ml X 3), the combined
organic layer was washed using water (20 ml X 2). The organic layer was
dried on anhydrous sodium sulphate and the solvent was removed under
reduced pressure to acquire the product. (Physical data of the synthesized
end products are summarized in the table 2.5.1)
Code
No.
Substitution
R1 & R2
Reaction Time
(min.) (at 480 W)
% Yield
DNJ-301 Piperidine 6.0 80
DNJ-302 Morpholine 6.3 84
DNJ-303 1-Methyl Piperazine 7.0 79
DNJ-304 1-Ethyl Piperazine 6.5 81
DNJ-305 1-Benzyl Piperazine 7.1 85
2.4.3 GENERAL PROCEDURE FOR THE PREPARATION OF DNJ-401 TO
DNJ-405
STEP – 1 GENERAL PROCEDURE FOR THE PREPARATION OF SIDE
CHAINS SC-06 TO SC-10
It was prepared according to the method described by Charles and
Sharma. b A solution of 0.01 mole chloroacetyl chloride in 40 ml dry benzene
was added drop wise to a cooled and stirred mixture of 0.01 mole an
appropriate secondary amine and 0.01 mole triethylamine in 40 ml dry
b E. S. Charles and S. Sharma; Ind. J. Chem., 1987, 26B(8), 752
Department of Chemistry, Saurashtra University, Rajkot – 360 005 80