反应详情

温度

180 °C

First, 14.8 g of diethyl 2,2-bis(6-benzyloxyhexyl)malonate, 0.5 g of water, 2.3 g of lithium chloride, and 50 ml of dimethyl sulfoxide were placed in a 100 ml flask. Then, the mixture was stirred at 180° C. for 12 hours. The reaction mixture was poured into water, and an organic layer was extracted with methylene chloride. The methylene chloride layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to obtain 9.4 g of ethyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 72.9%). The compound thus obtained had a purity of 97.9% by GC.

1. extractionan organic layer was extracted with methylene chloride
2. washThe methylene chloride layer was washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThereafter, the solvent was distilled away
5. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1)