反应详情

温度

-40 °C

Into a one liter, four-necked, round bottom flask equipped with stirrer, condenser, thermometer, and addition funnel, 25.3 parts of triethylamine, 17.2 parts of cyclopentanol, and 190.0 grams of methylene chloride were mixed under a nitrogen blanket and cooled to -40° C. with a dry ice-acetone bath. To this mixture 26.2 parts of methanesulfonyl chloride were added over one hour. The reaction mixture was stirred at -40° C. for an additional two hours and then allowed to warm to 0° C. and maintained at this temperature for eighteen hours. The mixture was vacuum filtered and then washed successively with chilled dilute sulfuric acid (twice with 200 part-portions), dilute sodium bicarbonate (three times with 200 part-portions), and water (twice with 200 part-portions). Subsequently the mixture was dried over sodium sulfate, filtered, and the solvent removed in vacuo to yield cyclopentyl methanesulfonate.

1. customInto a one liter, four-necked, round bottom flask equipped with stirrer, condenser
2. additionthermometer, and addition funnel
3. temperatureto warm to 0° C.
4. temperaturemaintained at this temperature for eighteen hours
5. filtrationfiltered
6. washwashed successively
7. temperaturewith chilled dilute sulfuric acid (twice with 200 part-portions), dilute sodium bicarbonate (three times with 200 part-portions), and water (twice with 200 part-portions)
8. dry with materialSubsequently the mixture was dried over sodium sulfate
9. filtrationfiltered
10. customthe solvent removed in vacuo