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

By Prof. L. Brandsma, Prof. H. D. Verkruijsse, Prof. S. F. Vasilevsky (auth.)

ISBN-10: 3540655506

ISBN-13: 9783540655503

ISBN-10: 3642603289

ISBN-13: 9783642603280

Homogeneous catalysis is a crucial procedure for the synthesis of high-valued chemical compounds. L. Brandsma has conscientiously chosen and checked the experimental strategies illustrating the catalytic use of copper, nickel, and palladium compounds in natural synthesis. All techniques are on a preparative scale, make fiscal use of solvents and catalysts, stay away from poisonous elements and feature excessive yields.

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3 mol (21 g, a large excess) of freshly distilled ethyl vinyl ether was added over 5 min. The solution was stirred for 10 min at -80°C, after which the temperature was allowed to rise over 15 min to -40 0c. 5 g) was added over 5 min at -60 to -70°C, after which the cooling bath was removed and the temperature allowed to rise to 0 0c. Water (100 ml) was added with vigorous stirring. The organic layer was dried over anhydrous MgS0 4 • Concentration in vacuo gave the product in almost 100% yield. If desired, the product can be distilled at a low pressure through a very short column.

10 molar (n-BuLi). Apparatus: 1-1 round-bottomed, three-necked flask, equipped with a nitrogen inletthermometer combination, an efficient mechanical stirrer and an outlet; during the addition of iodine the outlet was replaced with a powder funnel. 10 mol of n-butyllithiurn in 64 ml of hexane was added over a few min by syringe, while keeping the temperature of the solution at --70 DC by occasional cooling in a bath with liquid nitrogen. The temperature was allowed to rise to -40 DC, after which 200 ml of diethyl ether was added.

Equipped with a nitrogen inletthermometer combination, an efficient, gas-tight mechanical stirrer and a cold finger filled with dry ice and acetone (for the preparation of the hypobromite solution the flask was equipped with a dropping funnel, a mechanical stirrer and a thermometeroutlet combination). Procedure: (Cf. L. D. 60 mol, 96 g) was added over -15 min to a vigorously stirred solution of 90 g of potassium hydroxide (technical quality, -15% H 20) in 200 ml of water, while keeping the temperature between -5 and 0 DC (bath with dry ice and acetone).

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Application of Transition Metal Catalysts in Organic Synthesis by Prof. L. Brandsma, Prof. H. D. Verkruijsse, Prof. S. F. Vasilevsky (auth.)


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