反应详情

3.9 g of dimethyl 2-hydroxyethylphosphonate and 5.9 g of pyridine were dissolved in 40 ml. of dry diethyl ether, and the solution was cooled with ice to -5° C. A solution of 6.0 g of γ-bromopropylsulfonyl chloride in 30 ml. of dry diethyl ether was added dropwise to the cooled solution by means of a dropping funnel. After the addition, the mixed solution was allowed to stand for 24 hours at 0° to 5° C. The reaction mixture was poured into 50 ml. of 5% hydrochloric acid, and extracted with diethyl ether. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off at reduced pressure. The product was further dried at room temperature at 0.7 mmHg for 18 hours to afford dimethyl 2-(3-bromopropylsulfonyloxy)ethylphosphonate as a colorless oil in a yield of 75 mol %. The product showed the following characteristic values.

1. additionAfter the addition
2. additionThe reaction mixture was poured into 50 ml
3. extractionof 5% hydrochloric acid, and extracted with diethyl ether
4. dry with materialThe extract was dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off at reduced pressure
6. customThe product was further dried at room temperature at 0.7 mmHg for 18 hours