反应详情

First, 13.8 g of 2,2-bis(6-benzyloxyhexyl)ethanol, 10.2 g of triphenylphosphine, and 50 ml of methylene chloride were placed in a 200 ml flask. Then, 50 ml of a methylene chloride solution containing 16.1 g of carbon tetrabromide was added dropwise to the reaction mixture at room temperature, and the reaction mixture was stirred for 1 hour. The reaction mixture was washed with an aqueous solution of sodium bicarbonate and water in this order. The resultant reaction mixture was dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene) to obtain 11 g of 2,2-bis(6-benzyloxyhexyl)ethyl bromide (Y: 69%). The compound thus obtained had a purity of 97.5% by GC.

1. additionwas added dropwise to the reaction mixture at room temperature
2. washThe reaction mixture was washed with an aqueous solution of sodium bicarbonate and water in this order
3. customThe resultant reaction mixture
4. dry with materialwas dried over anhydrous sodium sulfate
5. distillationThereafter, the solvent was distilled away
6. customThe residue was purified by silica gel column chromatography (eluent: toluene)