反应详情

Into a 50 ml, round bottom, three-necked flask equipped with magnetic stirrer, pot thermometer, "Y" tube, nitrogen inlet tube, reflux condenser with cotton plug, and water bath is placed a solution of 0.65 grams (0.012 moles) of sodium methoxide dissolved in 10 ml anhydrous methanol. While maintaining the temperature of the reaction mass at 24°-27° C, a solution of 2.1 grams of 3-mercapto-2,6-dimethyl-4-heptanone dissolved in 12 ml anhydrous methanol is added to the sodium methoxide solution. 1.78 grams of 3-chloro-4-heptanone is then added to the reaction mass with stirring over a period of 2 minutes, the reaction mass temperature rising to 38° C. Two ml anhydrous methanol used as rinse is then added to the reaction mass, and with stirring the reaction mass temperature cools to 25° C. The reaction mass is continued to be stirred at 25° C for a period of 5 hours. At this point 25 ml distilled water is added, and the resulting solid dissolves. The oil phase is extracted with three 15 ml portions of methylene chloride, and the extracts are combined and washed with one 10 ml portion of water. The extracts are then dried over anhydrous sodium sulfate and gravity filtered and concentrated on a rotary evaporator using water aspirator vacuum to a weight of 3.20 grams (yellow oil). GLC analysis (8 feet × 1/4 inch SE-30 column), NMR, IR and mass spectral analyses of GLC isolated material yield the information that the resulting product is 85% pure and has the structure: ##STR56##

1. customInto a 50 ml, round bottom, three-necked flask equipped with magnetic stirrer
2. temperatureWhile maintaining the temperature of the reaction mass at 24°-27° C
3. customrising to 38° C
4. washas rinse
5. additionis then added to the reaction mass
6. stirringwith stirring the reaction mass temperature
7. customcools to 25° C
8. stirringto be stirred at 25° C for a period of 5 hours
9. distillationAt this point 25 ml distilled water
10. additionis added
11. dissolutionthe resulting solid dissolves
12. extractionThe oil phase is extracted with three 15 ml portions of methylene chloride
13. washwashed with one 10 ml portion of water
14. dry with materialThe extracts are then dried over anhydrous sodium sulfate and gravity
15. filtrationfiltered
16. concentrationconcentrated on a rotary evaporator
17. customGLC analysis (8 feet × 1/4 inch SE-30 column), NMR, IR and mass spectral analyses of GLC isolated material
18. customyield the information that the resulting product