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

HRID 2418321

반응식

HRID 2418321 반응식
C1(C)[CH:6]=[CH:5][C:4]([S:7](O)(=O)=O)=CC=1.[CH2:12]([SH:16])[CH:13]([SH:15])C.[CH3:17]CC=S>C1CCCCC1>[CH3:6][CH:5]1[CH2:4][S:7][CH:13]([CH2:12][S:16][CH3:17])[S:15]1

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 612172,3-DimercaptopropaneHCID 138345Propanethial

생성물 1

HCID 218808374-Methyl-2-[(methylsulfanyl)methyl]-1,3-dithiolane

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-984d4c1b9bf947c09f62b8adafccbb82
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472446

연결된 노트

불러오는 중…