Application of Transition Metal Catalysts in Organic by L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse

April 3, 2017 | Organic | By admin | 0 Comments

By L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse

Homogeneous catalysis is a crucial technique 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 tactics are on a preparative scale, make financial use of solvents and catalysts, stay away from poisonous elements and feature excessive yields.

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The compound is stable at room temperature. 2 ppm. Notes: 1. Since contact of the skin with 35% hydrogen peroxide causes very painful white spots, protection of skin and eyes is essential. 2. If too much of hydrogen peroxide is added at low temperatures, the reaction may become very vigorous and no longer controllable at somewhat higher temperatures. Temperature observation after each addition therefore is absolutely necessary. 5-Dibromothiophene o 48 + (/r· aq. II Br 2Br2 D .. 50 molar (thiophene).

05 (2H) ppm. 50 molar. Apparatus: I-I round-bottomed, three-necked flask, equipped with a nitrogen inletthermometer combination, an efficient mechanical stirrer and a reflux condenser; for the iodination the condenser was replaced by a powder funnel. 50 mol n-butyllithium in 320 ml of hexane was placed in the flask. The hexane was removed by evacuation (water aspirator) and heating the flask in a bath at 30 to 40°C. To the remaining viscous liquid was added 300 ml of cold (-30°C), dry diethyl ether.

20 ~ +40 °C • Scale: 3 molar (thiophene). Apparatus: 2-1 round-bottomed, three-necked flask, equipped with a dropping funnel, an efficient mechanical stirrer and a thermometer-outlet combination. 5 mol) and 100 ml of diethyl ether. 0 mol, was added in portions of 25-30 ml from the dropping funnel, while cooling the flask in a bath with dry ice and acetone. After addition of each portion the solution became temporarily light-brown. Initially, the temperature of the efficiently stirred mixture was kept between -10 and -20°C, but as the heating effect caused by further additions became less strong, the temperature of the mixture was gradually raised to between +10 and 20°C (see Note 2).

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