Furfural → 2-(2-Furyl)-4-Methyl-1,3-Dithiolane

Into a 100 ml reaction flask equipped with reflux condenser, thermometer and magnetic stirring bar and hot plate with magnetic stirring apparatus is placed 0.5 grams paratoluenesulfonic acid, 5 ml cyclohexane and 5.4 grams (0.05 moles) of 1,2-propanedithiol. Over a period of 25 minutes with stirring is added 4.8 grams (0.05 moles) of 2-furaldehyde. The reaction mass is then heated to reflux and refluxed for a period of 8 hours while removing water of reaction. At the end of the refluxing period, the reaction mass is cooled to room temperature and transferred to a separatory funnel. The reaction mass is washed with one 50 ml portion of aqueous saturated sodium chloride, and dried over anhydrous sodium sulfate. The reaction mass is then filtered and the filtrate is distilled on a Microvigreux column yielding the following three fractions:

1. customInto a 100 ml reaction flask
2. customequipped
3. temperaturewith reflux condenser
4. customthermometer and magnetic stirring bar and hot plate with magnetic stirring apparatus is placed
5. temperatureThe reaction mass is then heated
6. temperatureto reflux
7. temperaturerefluxed for a period of 8 hours
8. customwhile removing
9. customwater of reaction
10. customtransferred to a separatory funnel
11. washThe reaction mass is washed with one 50 ml portion of aqueous saturated sodium chloride
12. dry with materialdried over anhydrous sodium sulfate
13. filtrationThe reaction mass is then filtered
14. distillationthe filtrate is distilled on a Microvigreux column
15. customyielding the following three fractions

ORDレコード

ord-7b99e9dbc04e4b29ba4eeb3783963375

出典データセット

uspto-grants-1985_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04515968