Synthesis of aluminum isopropoxide "Preparation of aluminum isopropoxide"

Synthesis of aluminum isopropoxide

Aluminum isopropoxide is a useful reagent in organic chemistry. It mainly oxidizes secondary alcohols to ketones, or reduces ketones or aldehydes to alcohols in the opposite direction. According to the opposite direction, the reaction has different names. If ketones are reduced to alcohols, it is called Millwin Pendulum Weilei reduction, abbreviated as MPV reduction, but if alcohols are oxidized, it is called Woo type oxidation reaction. The direction of the reaction only depends on the raw material. We will use the product for MPV reduction synthesis of 1-octen-3-ol (mushroom alcohol), which is a chemical attractant for biting insects.

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Preparation of aluminum isopropoxide

The commonly used method for preparing isopropanol aluminum was developed in 1936, which involves heating and refluxing a mixture of 100g of aluminum, 1200mL of isopropanol, and 5g of mercury chloride. Trace amounts of iodine can be added as an initiator. The reaction generated aluminum amalgam. After distillation and purification at 140-150 ° C and 5mmHg, Young et al. achieved yields of 85-90% In addition, carbon tetrachloride can also be used instead of mercury chloride or iodine, as follows: prepared by reacting metal aluminum with isopropanol under the catalysis of mercury chloride.

Place 1mol of aluminum wire or aluminum sheet in a 1L flask equipped with a reflux condenser and calcium chloride drying tube. 300mL of anhydrous isopropanol can be obtained by distillation with industrial isopropanol and 5% of its mass sodium. And 0.5g HgCl2. heat reflux, add 2mL of carbon tetrachloride through the condenser when boiling begins, continue heating, and guide the sudden release of hydrogen gas. Remove heat sources and sometimes require cooling.

After the intense reaction has calmed down, continue to boil until the aluminum has completely reacted (about 6-12 hours), evaporate the solvent, and then perform vacuum distillation on the remaining product. Collect the product with a boiling point of 130-140 ℃/933Pa (7mmHg). The yield ranges from 90% to 95%. The product usually takes 1-2 days to solidify and can be stored in a glass bottle sealed with paraffin.

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