By L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse
Homogeneous catalysis is a crucial process for the synthesis of high-valued chemical compounds. L. Brandsma has conscientiously chosen and checked the experimental tactics illustrating the catalytic use of copper, nickel, and palladium compounds in natural synthesis. All approaches are on a preparative scale, make financial use of solvents and catalysts, keep away from poisonous ingredients and feature excessive yields.
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Additional info for Application of Transition Metal Catalysts in Organic Synthesis (Springer Laboratory)
15 ppm. Note: For precautions when working with hydrogen peroxide see expo in Sect. l. 6 molar. Apparatus: 1-1 round-bottomed, three-necked flask, equipped with a mechanical stirrer and two outlets for the preparation of sodamide; 2- or 3-1 round-bottomed, threenecked flask, equipped with two outlets and a mechanical stirrer for the disproportionation reaction. Procedure: (See also 1. D. Verkruijsse, Synth. Comm. ) Anhydrous liquid ammonia (see Note 1) (-500 ml) was introduced from a cylinder into the first flask.
Yokomatsu, S. Shibuya, Heterocyel. 22 mol (24 g) of diisopropylamine and 120 ml ofTHF, while keeping the temperature between 0 and -20°C (cooling in a bath with nitrogen allows a quick addition by syringe). 4 g) of 2,5-dibromothiophene was added in one portion. The temperature was allowed to rise to -10 °C (a purple solution was formed) at which level stirring was continued for an additional 15 min. The dark mixture was then poured into 500 ml of an aqueous solution of 30 g of ammonium chloride.
The solution was stirred for an additional 15 min at 0 DC, then it was cooled to below -55 DC. 9 g) was introduced portionwise over 15 min, while keeping the temperature around -40 DC. After the addition the temperature was allowed to rise to 0 DC. The mixture was then treated with a solution of 10 g of Na2S203·5H20 in 100 ml of water under vigorous stirring. 5 mmHg). The remaining solid was purified by crystallization from diethyl ether. 1-Bromo-4-iodo-benzene was obtained in greater than 80% yields.