Benzaldehyde → 4,5-Dimethyl-2-Phenyl-1,3-Dithiolane

HRID 462575

反応式

HRID 462575 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4](S(O)(=O)=O)=[CH:3][CH:2]=1.C1CCCCC1.[CH3:18][CH:19]([SH:23])[CH:20]([SH:22])[CH3:21].C(=O)C1C=CC=CC=1>O>[CH3:21][CH:20]1[CH:19]([CH3:18])[S:23][CH:11]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[S:22]1

参加物

6

反応物 4

HCID 240BenzaldehydeHCID 6101p-Toluenesulfonic acidHCID 8078CyclohexaneHCID 5483532,3-Butanedithiol

生成物 1

HCID 203986774,5-Dimethyl-2-Phenyl-1,3-Dithiolane

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a 100 ml reaction flask equipped with thermometer, reflux condenser and magnetic stirring bar and hot plate with magnetic stirring apparatus is placed 0.5 grams of para-toluenesulfonic acid, 5.0 ml cyclohexane and 6.1 grams (0.05 moles) of 2,3-butanedithiol. Over a period of 25 minutes, 5.3 grams (0.05 moles) of benzaldehyde is added to the reaction mass with stirring. The reaction mass is then heated to reflux with stirring and refluxed for a period of 9.5 hours while taking off 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 then washed with one 50 ml portion of saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled on a Microvigreux column yielding the following three fractions:

後処理

  1. customInto a 100 ml reaction flask
  2. customequipped with thermometer
  3. temperaturereflux condenser and magnetic stirring bar
  4. temperatureThe reaction mass is then heated
  5. temperatureto reflux
  6. stirringwith stirring
  7. temperaturerefluxed for a period of 9.5 hours
  8. customtransferred to a separatory funnel
  9. washThe reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution
  10. dry with materialdried over anhydrous sodium sulfate
  11. filtrationfiltered
  12. distillationThe resulting filtrate is distilled on a Microvigreux column
  13. customyielding the following three fractions

出典と根拠

ORDレコード
ord-677da6f870204dd18eaecd4cabad47c2
出典データセット
uspto-grants-1985_05
特許番号
US04515968

関連ノート

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