09/01/2012 LABORATORY REPORT BY OKEMWA EVANS KENANDA

1.1 SYNTHETIC MODIFICATION OF 6 -HYDROXY-2 ,4 DIMETHOXYCHALCONE (JMN 10 or 201) 1.1.1 Synthesis of Pyrazolines 1. OEK-03-1
H3CO OCH3 NH2OH.HCl OH O 4 hours OH N O H3CO OCH3

White solid

Mass of substrate Mass of OEK-07-1 Mass of OEK-M7 Other compounds OEK-06-1

= 100mg = 0.029g =

A mixture of 6 -hydroxy-2 ,4 dimethoxychalcone, (0.355mg), phenyl hydrazine (50mmol) and ethanol (60ml) was heated at reflux for 4 hrs, and then poured onto crushed ice. The precipitate formed was separated by filtration, washed with water, and crystallized from methanol. A fibre-like whitish yellow a solid (suspected to the pyrazoline) was obtained.
H3CO OCH3 H3CO NH2NHPh, refluxing OH O 4 hours OH N N OCH3

A very white fibre-like compound recrystallized from motherliquor OEK-M4 after three days of standing. Mass of OEK-61 = 0.00041g

1.2 SYNTHETIC MODIFICATION OF JMN-7 Oek-08-1(synthesis of pyrazoline from JMN7) - Reagent: Hydrazine hydrate -Re-crystallized from methanol as a black solid Mass of sample JMN-10 =200g Mass of OEK-08-1 = 0.0742 Mass of OEK-M7 (motherliquor) = 0.1731g

whitish yellow solid

Mass of substrate = 0.355g Mass of OEK-03-1 = 0.0783g Mass of motherliquor (OEK M31) = 0.160g 2. OEK-04-1 = OEK-04-2 (synthesis of pyrazoline from JMN-10) Reagent: Hydrazine hydrate Re-crystallized as A yellow powder
H3CO OCH3 H3CO NH2NH2.H2O OH O 4 hours OH HN N OCH3

Yellow solid

Mass of substrate Mass of OEK-04-1 Mass of motherliquor (OEK M4

= 0.1g = 0.0526 =

Synthesis of isoxazolines from JMN-10 Reagent : NH2OH.HCl OEK-07-1 -white solid re-crystallized from ethanol.

OEK-09-1 (synthesis of pyrazoline from JMN7) - re-crystallized from methanol as a white solid Reagent: phenylhydrazine Mass of substrate =0.2000g Mass of OEK-09-1 = 0.1455 Mass of OEK-M7(motherliquor) = TOTAL NO. OF PRODUCTS = 6

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