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Questions And Answer

• Preparation

  1) Add 197 g of D-camphor to a four-necked flask, then add 500 g of diethyl ether, 63 g of magnesium shavings, and 1 mg of elemental iodine sequentially at room temperature to obtain mixed system A;

  2) Slowly add 295 g of iodomethane dropwise to mixed system A at room temperature, keeping the reaction temperature below 20°C during the dropwise addition. After the dropwise addition is complete, stir the above reaction solution at room temperature for 2 hours, then heat and reflux for 7 hours. After gas chromatography shows that the raw materials have reacted completely, cool and filter.

  The solid obtained after filtration was discarded. The solution was diluted with 150 mL of petroleum ether, washed with 150 mL of 2M hydrochloric acid solution, and allowed to stand for separation. The organic and aqueous phases were then separated, and the aqueous phase was discarded. The organic phase was washed with 150 mL of saturated brine, and the organic and aqueous phases were then separated, and the aqueous phase was discarded. The organic phase was mixed with 150 mL of a solution containing 30 g of hydroxylamine hydrochloride and 30 g of sodium hydroxide, stirred at room temperature for 30 hours, separated, and the aqueous phase was discarded. The organic phase was dried with anhydrous sodium sulfate, and the solvent was removed by rotary evaporation to obtain 216 g of crude product.

  3) The above crude product was recrystallized with a mixed solvent of 500 g of water and 1200 g of ethanol to obtain 178 g of product 2-methylisoborneol, with a yield of 82% and a purity >98%.

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