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3.8. Experimental protocols
3.8.1 General Procedure for the Preparation of hydroxy Salts. (Microwave)
According to process described in chapeter-2 40 new hydrocy salts were
synthesized
3.8.2 General Procedure for the Preparation of HClO4 Salts.
A mixture of 84% polyphosphoric acid (3 g) and hydroxy salts (3 mmol) was heated
in 50 ml beaker upon intensive stirring at 150 °C for 15 min. After cooling to the
room temperature the resulting viscous mass was dissolved in 30 ml of water and 1 ml
(10 mmol) of 70% HClO4 was added dropwise upon mild stirring. The white
precipitate was washed with distilled water (3×10 mL), ether (2×10 mL) until a
neutral reaction of the pH paper and then dried over P2O5 to give salt as fine white
crystals.
In similar manner 40 new compounds were synthesized.
3.8.3 General Procedure for the Microwave-Assisted Synthesis of 2aminoimidazoles.
To a suspension of HClO4 salt (2 mmol) in MeCN (5 mL) hydrazine hydrate (0.7 mL,
14 mmol of a 64% solution, 7 equiv) was added, and the mixture was irradiated in the
sealed Milestone MicroSYNTH microwave reactor for 10 min at a ceiling
temperature of 100 °C at 150 W maximum power. After cooling down the reaction
was worked up by diluting with DCM (300 mL), washing with sat. NH4Cl solution
(150 mL), brine (150 mL) and water (2×150 mL) and drying over anhydrous Na2SO4.
After filtration and concentration the resulting residue was purified by column
chromatography (silica gel; DCM−MeOH, 9:1 v/v with 3% TEA) to afford the
product as a colourless solid.
40 new compounds were synthesized In similar manner.