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Chapter – 5 Synthesis and Characterization…..
5.8 EXPERIMENTAL
5.8.1 PREPARATION OF 4-HYDROXY COUMARIN
It was prepared according to the method reported by Shah et. al. a Yield
- 55 %, MP - 210-212°C (210-212°C a ).
5.8.2 GENERAL PROCEDURE FOR THE PREPARATION OF 4-
(SUBSTITUTED ANILINO) COUMARIN
Mixture of 0.1 mole of 4-hydroxy coumarin and 0.1 mole of
appropriately substituted primary amine was irradiated neat under microwave
irradiation using domestic microwave oven (LG MS-192 W) for desired time at
320 Watt. The reaction mixture was cooled to room temperature and
methanol was added to it. The separated solid was filtered and washed with
methanol. It was dried and recrystallized with dimethylformamide to give 4-
(substituted anilino) coumains. Required reaction time and obtained results
are summarized as under.
Code No.
Reaction
Time (min.)
320 Watt
% yield Code No.
Reaction
Time (min.)
320 Watt
% yield
AAC-1 6.0 81 AAC-8 6.4 91
AAC-2 4.1 85 AAC-9 5.3 83
AAC-3 6.3 79 AAC-10 7.3 80
AAC-4 5.2 88 AAC-11 7.1 79
AAC-5 5.5 84 AAC-12 7.0 88
AAC-6 4.3 90 AAC-13 5.2 84
AAC-7 6.2 77
a A. K. Shah, N. S. Bhatt and V. M. Thakor; Curr. Sci., 1984, 53(24), 1289.
Department of Chemistry, Saurashtra University, Rajkot – 360 005 294