Propylene Glycol → 1,3-Dioxolane, 4-methyl-2-[2-(methylthio)ethyl]-

HRID 462568ノート

反応式

HRID 462568 の反応式
[CH2:1]1[CH2:6][CH2:5]CCC1.C1(C)C=C[C:10]([S:13](O)(=O)=O)=CC=1.[CH2:18]([OH:22])[CH:19]([OH:21])[CH3:20].CCCC=S>O>[CH3:20][CH:19]1[CH2:18][O:22][CH:1]([CH2:6][CH2:5][S:13][CH3:10])[O:21]1

参加物

6

反応物 4

HCID 1030Propylene GlycolHCID 6101p-Toluenesulfonic acidHCID 8078CyclohexaneHCID 12463483Butanthial

生成物 1

HCID 1009271,3-Dioxolane, 4-methyl-2-[2-(methylthio)ethyl]-

試薬・触媒・溶媒 1

HCID 962Water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 3.8 grams (0.05 moles) of 1,2-propanediol. Over a period of 8 hours, 3-methylthiopropionaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and during refluxing water of formation is removed. The refluxing continues for a period of 7 hours. At the end of the 7 hour period, the reaction mass is transferred to a separatory funnel and washed with one 50 ml portion of saturated aqueous sodium chloride solution and 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. customis removed
  8. waitThe refluxing continues for a period of 7 hours
  9. customAt the end of the 7 hour period, the reaction mass is transferred to a separatory funnel
  10. washwashed with one 50 ml portion of saturated aqueous sodium chloride solution
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationfiltered
  13. distillationdistilled on a Microvigreux column
  14. customyielding the following fractions

出典と根拠

ORDレコード
ord-dee058d289184193a15c03ac9d87f9af
出典データセット
uspto-grants-1985_05
特許番号
US04515966

反応ノート

読み込み中…