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Ethylene Glycol → 2-[2-(Methylsulfanyl)ethyl]-1,3-dioxolane

HRID 462569
ノート
印刷プレビュー

反応式

HRID 462569 の反応式
C1(C)[CH:6]=[CH:5][C:4]([S:7](O)(=O)=O)=CC=1.[CH2:12]([OH:15])[CH2:13][OH:14].[CH3:16]CCC=S>C1CCCCC1>[CH3:16][S:7][CH2:4][CH2:5][CH:6]1[O:15][CH2:12][CH2:13][O:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 12463483Butanthial

生成物 1

HCID 203986662-[2-(Methylsulfanyl)ethyl]-1,3-dioxolane

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

Into a 100 ml reaction flask equipped with spin bar, reflux condenser, heating mantle and hot plate with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams para-toluenesulfonic acid and 3.1 grams (0.05 moles) of 1,2-ethanediol. Over a period of 30 minutes, 5.2 grams (0.05 moles) of 3-methylthiopropionaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and during reflux, water of formation is removed. The refluxing continues for a period of 9 hours. At the end of the 9 hour period, the reaction mass is cooled and transferred to a separatory funnel and washed with one 50 ml portion of saturated sodium chloride solution. The reaction mass is then dried over anhydrous sodium sulfate, filtered and distilled on a Microvigreux column yielding the following fractions:

後処理

  1. customInto a 100 ml reaction flask
  2. customequipped with spin bar
  3. temperaturereflux condenser
  4. temperatureheating mantle
  5. temperatureThe reaction mass is then heated
  6. temperatureto reflux
  7. temperatureduring reflux
  8. customwater of formation is removed
  9. waitThe refluxing continues for a period of 9 hours
  10. temperatureAt the end of the 9 hour period, the reaction mass is cooled
  11. customtransferred to a separatory funnel
  12. washwashed with one 50 ml portion of saturated sodium chloride solution
  13. dry with materialThe reaction mass is then dried over anhydrous sodium sulfate
  14. filtrationfiltered
  15. distillationdistilled on a Microvigreux column
  16. customyielding the following fractions

出典と根拠

ORDレコード
ord-15e0e6d7877e4a7fb44a6ac360eda85b
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04515966

反応ノート

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