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Chapter – 4 Studies on different types of reactions….. 4.8.3 SCHEME - 3 X N N H N N N O NH2 4.8.4 SCHEME - 4 H O O O H O O + H O O N N H + H + N N R NH + X N N NH 2 + X O H N OH + H H N N H O NH2 H O O O Department of Chemistry, Saurashtra University, Rajkot – 360 005 223 O O O O H OH H N N - H 2 O N N R OH C + H N N X H H N + + H + OH N H : N N NH N H 2 X O NH 2 O O O X NH 2 O N N R
Chapter – 4 Studies on different types of reactions….. 4.9 EXPERIMENTAL 4.9.1 PREPARATION OF PYRAZOLE ALDEHYDE STEP – 1 PREPARATION OF ACETOPHENONE PHENYL HYDRAZONE 0.1 mole of appropriately substituted acetophenone was dissolved in 50 ml of ethanol into 250 ml round bottom flask. 0.1 mole of Phenyl hydrazine was added to above flask along with 3-4 drops of glacial acetic acid. The reaction mixture was refluxed for 5-6 hours. 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 a mobile phase. After the reaction to be completed, the reaction mixture was cooled to room temperature and the crystalline product was separated by filtration. The product was washed with ethanol and dried to give substituted acetone phenyl hydrazone in good yield which was pure enough to use as such for the next step. Code No. MF MW (g/m) MP (°C) % Yield APH-01 C14H13N3O2 255 106-108 85 APH-02 C14H13N3O2 255 134-136 80 APH-03 C14H14N2 210 126-128 78 APH-04 C14H13ClN2 244 ----- 79 APH-05 C14H13FN2 228 ----- 72 STEP – 2 PREPARATION OF PYRAZOLE ALDEHYDE 25 ml of dry dimethylformamide was transferred into 250 ml flat bottom flask. 3 ml of phosphorous oxychloride was added drop wise to above flask under stirring at 0-5°C. After completion of the addition, the mixture was stirred at this temperature for 10-15 min. 0.03 mole of freshly prepared acetophenone phenyl hydrazone was added to above mixture and the content was heated on water bath for 5-6 hours. 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 a mobile phase. After the reaction to be completed, the reaction mixture was cooled to room temperature and the Department of Chemistry, Saurashtra University, Rajkot – 360 005 224
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Saurashtra University Re - Accredit
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Statement under O. Ph. D. 7 of Saur
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ACKNOWLEDGEMENT It is a moment of g
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Jignesh Lunagariya, Hitesh Sarvaiya
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CONTENT Content General Remarks 6 A
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Content 3.2 Reaction scheme 149 3.3
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5.14 Conclusion 313 5.15 Spectral r
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MF Molecular Formula MW Molecular W
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GABA Gamma Amino Butyric Acid MES M
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PART - A STUDIES ON 2-METHYL INDOLI
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Part-A Studies on 2-methyl indoline
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CHAPTER - 1 PREPARATION AND YIELD O
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Chapter - 1 Preparation and Yield o
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Chapter - 2 Microwave assisted simp
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Part - B Studies on isatin derivati
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CHAPTER - 3 PREPARATION OF SMALL LI
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Chapter - 3 Preparation of small li
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Chapter - 4 Studies on different ty
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Chapter - 4 Studies on different ty
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Chapter - 5 Synthesis and Character
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Chapter - 6 Biological evaluation o
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Summary Synthesis and biological pr
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Summary Synthesis and biological pr
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Conferences / Seminar / Workshop At
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