Oleamide CAS 301-02-0

Approach 1: Oleic acid (25g, 74% pureness) was billed right into a 250ml round base flask, and also strong urea beads (22g) were billed into the exact same flask together with tetrabutyl titanate (0.25 g). The blend was stirred for one minute with a magnetic stirrer in a 900W microwave dental caries. The heating program raised the temperature from ambient to 190 ° C within 5 min and also held at 190 ° C for an extra 25 min. During home heating, urea will certainly melt above 135 ° C and begin to decompose at 150 ° C launching NH3 and carbon dioxide. The acid variety of the response item was identified to be around 10, as well as the conversion of oleic acid to the reaction product was about 95% based on the acid number. The cooled down reaction product from Instance 1 was blended with chloroform as well as any type of unreacted urea was filtered from the reaction product. The chloroform fraction was then evaporated on a rotating evaporator to manage Oleamide. The yield of Oleamide is 92%, melting point 74 ° C. The artificial course is shown in Figure 1.

Technique 2: Consider 25 grams of reactant (Z)-octadecenoic acid. Place it right into a 500mL four-port response vessel. The mixture was dried out at 280 ° C for 16 hrs. Include 350 mL of dichloroethylene (CH2Cl2) to the reaction combination. Stirring was continued for thirty minutes and the blend was cooled to 0-5 ° C. Twenty-two milliliters of oxalyl chloride was added in small amounts to the reaction blend. Raise the temperature over 5 ° C. The reaction combination was reacted at area temperature level for 4 hrs. Full the reaction. Location the combination under vacuum cleaner. Excess CH2Cl2 and also oxalyl chloride were vaporized. The reaction vessel was restored with fresh CH2Cl2 (250 mL). Refrigerate the option to 0-5 ° C. A stream of ammonia [NH3(g)] was contributed to the response vessel for 1 hour. The mixture was evaporated in vacuo to completely eliminate excess CH2Cl2. Ethyl acetate (500 mL) was added to dissolve the deposit. After rinsing the remedy with 300 mL of distilled water, the ethyl acetate layer was separated. Laundry the ethyl acetate layer with 200 mL of saturated sodium bicarbonate (NaHCO3) solution and adequate distilled water to get a neutral pH. The remedy was dehydrated with sufficient anhydrous magnesium sulfate. Filter the service. The filtrate was vaporized in vacuo to completely remove ethyl acetate. The crude item was detoxified on a C-18 column chromatography (i.d.x l=1.5 x 24 centimeters) utilizing a mixed mobile phase (acetonitrile/HO=80:20) operating at 3 mL/min to obtain the highly pure substance Oleamide. The artificial path is displayed in Figure 1.