By L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse
Homogeneous catalysis is a crucial process for the synthesis of high-valued chemical substances. L. Brandsma has rigorously chosen and checked the experimental strategies illustrating the catalytic use of copper, nickel, and palladium compounds in natural synthesis. All approaches 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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Extra info for Application of Transition Metal Catalysts in Organic Synthesis (Springer Laboratory)
Most of the solvent was distilled off at atmospheric pressure through a 40-cm Vigreux column. After cooling to room temperature, the remaining liquid was subjected to careful distillation through a 30 or 40-cm Widmer column. 2Bromothiophene was collected at between 40 and 80 °C115 mmHg. A small amount (between 10 and 25 g) of2,5-dibromothiophene passed over between 80 and 105°C/IS mmHg. p. 5868, in 80% or higher yields. 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.
493, in -75% yield. The compound is fairly stable at room temperature. 5 molar. D DMF 30-35°C • Br 0 + 2HBr Br 32 2 Procedures for the Preparation of Halogen Compounds Apparatus: 1-1 round-bottomed, three-necked flask, equipped with a dropping funnel, a mechanical stirrer and a thermometer-outlet combination. A. J. Klomp, 1. Brandsma, Synth. Comm. 50 mol (34 g) of freshly distilled furan and 240 ml of N,N-dimethylformamide. During the addition the temperature of the mixture was kept between 30 and 35°C.
The temperature of the mixture, initially kept between -5 and +5 DC, was raised to -20°C towards the end of the addition. After disappearance of the brown colour caused by bromine, the layers were separated. The upper layer was extracted four times with very small portions of dichloromethane (see Note). The combined organic solutions were washed with water, dried over anhydrous magnesium sulfate (or vigorously shaken with the smallest possible amount of phosphorus pentoxide), and then concentrated under reduced pressure.
Application of Transition Metal Catalysts in Organic Synthesis (Springer Laboratory) by L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse