反应详情

温度

33 °C

Into a 50 ml round bottom 1 neck flask equipped with nitrogen inlet tube, "Y" tube, reflux condenser, magnetic stirrer, and cold water bath is placed a solution containing 0.54 g of sodium methylate (0.01 moles) in 6 ml of anhydrous methanol. 1.14 g (0.01 moles) of 2-methyl-3-furan thiol in 6 ml of anhydrous methanol is then added to the sodium methylate solution. The reaction mass is stirred for a period of 10 minutes, with cooling, maintaining the temperature thereof between 24° and 30° C. 0.91 g (0.01 moles) of a mixture of 80% 1-chloro-2-butene and 20% 3-chloro-1-butene dissolved in 2 ml of anhydrous methanol is then added over a 4 minute period warming to 33° C. The reaction mass is allowed to cool to 23° C. and remains at that temperature, with stirring, for a period of 2.5 hours, at which time it is concentrated to 7 ml on a rotary evaporator using water aspirator vacuum. 20 ml water is then added and the reaction mass is neutralized to a pH of 5 - 6 using 4% hydrochloric acid. The reaction mass is extracted with three 10 ml portions of n-hexane. The hexane extracts are combined, washed with 2 ml saturated sodium chloride solution, dried with anhydrous sodium sulfate and concentrated using a rotary evaporator to yield 1.24 g of a yellow oil.

1. customInto a 50 ml round bottom 1 neck flask equipped with nitrogen inlet tube
2. temperature"Y" tube, reflux condenser, magnetic stirrer, and cold water bath
3. temperaturewith cooling
4. temperaturemaintaining the temperature
5. custombetween 24° and 30° C
6. additionis then added over a 4 minute period
7. temperatureto cool to 23° C.
8. stirringwith stirring, for a period of 2.5 hours, at which time it
9. concentrationis concentrated to 7 ml on a rotary evaporator
10. addition20 ml water is then added
11. extractionThe reaction mass is extracted with three 10 ml portions of n-hexane
12. washwashed with 2 ml saturated sodium chloride solution
13. dry with materialdried with anhydrous sodium sulfate
14. concentrationconcentrated
15. customa rotary evaporator