p-Toluenesulfonic acid → 4-Methyl-2-[(methylsulfanyl)methyl]-1,3-dithiolane

Into a 100 ml reaction flask equipped with reflux condensor, heating mantle, hot plate equipped with magnetic stirring apparatus and magnetic stirring bar is placed 10 ml cyclohexane, 0.5 grams of para toluene sulfonic acid and 10.8 grams (0.1 mole) of 1,2-propanedithiol. Over a period of one hour, 9 grams (0.1 mole) of methylthioacetaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and maintained at reflux for a period of eight hours. At the end of the eight hour period the reaction mass is transferred to a separatory funnel and washed with one 50 ml portion of a saturated aqueous sodium chloride solution, then dried over anhydrous sodium sulfate, filtered and distilled. The distillation takes place on a micro vigreux column yielding the following fractions:

1. customInto a 100 ml reaction flask
2. customequipped
3. temperaturewith reflux condensor
4. temperatureheating mantle
5. customhot plate equipped with magnetic stirring apparatus and magnetic stirring bar
6. temperatureThe reaction mass is then heated
7. temperatureto reflux
8. temperaturemaintained
9. temperatureat reflux for a period of eight hours
10. customAt the end of the eight hour period the reaction mass is transferred to a separatory funnel
11. washwashed with one 50 ml portion of a saturated aqueous sodium chloride solution
12. dry with materialdried over anhydrous sodium sulfate
13. filtrationfiltered
14. distillationdistilled
15. distillationThe distillation
16. customyielding the following fractions

ORDレコード

ord-faeb3390626a40d5b2a3f7bb4e8f6a9e

出典データセット

uspto-grants-1985_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04515967