Phenylacetaldehyde → HCID 20398674、化合物

HRID 462573

反応式

HRID 462573 の反応式
C1CCCCC1.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:18]([SH:22])[CH:19]([SH:21])[CH3:20].[C:23]1([CH2:29][CH:30]=O)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>O>[CH2:29]([CH:30]1[S:21][CH:19]([CH3:20])[CH2:18][S:22]1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

6

反応物 4

HCID 998PhenylacetaldehydeHCID 6101p-Toluenesulfonic acidHCID 8078CyclohexaneHCID 612172,3-Dimercaptopropane

生成物 1

HCID 20398674HCID 20398674、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a 100 cc reaction flask equipped with reflux condenser, magnetic stirring bar and thermometer and hot plate equipped with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams of para-toluenesulfonic acid and 5.4 grams (0.05 moles) of 1,2-propanedithiol. With stirring, over a period of 30 minutes, 6 grams (0.05 moles) of phenylacetaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and refluxed for a period of 8 hours. During the refluxing period, water of reaction is removed. 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 cc reaction flask
  2. customequipped
  3. temperaturewith reflux condenser, magnetic stirring bar
  4. customthermometer and hot plate equipped with magnetic stirring apparatus
  5. temperatureThe reaction mass is then heated
  6. temperatureto reflux
  7. temperaturerefluxed for a period of 8 hours
  8. customis removed
  9. customtransferred to a separatory funnel
  10. washThe reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationfiltered
  13. distillationThe resulting filtrate is distilled on a Microvigreux column
  14. customyielding the following three fractions

出典と根拠

ORDレコード
ord-b2aec404a6724b75be1cceecbe7a91ce
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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