Benzene → 1,3-Dithiane-2-carboxylic acid

HRID 268322

反応式

HRID 268322 の反応式
[OH2:1].[CH2:2]([SH:6])[CH2:3][CH2:4][SH:5].C1(C)C=CC(S(O)(=O)=[O:14])=CC=1.[CH:18]1[CH:23]=CC=CC=1>>[S:5]1[CH2:4][CH2:3][CH2:2][S:6][CH:23]1[C:18]([OH:14])=[O:1]

参加物

5

反応物 4

HCID 241BenzeneHCID 962Water2 回HCID 6101p-Toluenesulfonic acidHCID 80131,3-Propanedithiol

生成物 1

HCID 3037051,3-Dithiane-2-carboxylic acid

実験手順

In a one liter three-necked reaction flask equipped with a water-separator device (Dean-Stark) and a reflux condenser there are added 700 ml. of benzene, 54 g (0.5 mol) of 1,3-propanedithiol 46 g (0.5 mol) of monohydrated glyoxylic acid and 0.5 g (2.9 mmol) toluene-p-sulfonic acid. The mixture is heated to reflux with stirring. After 18 ml. (1 mol) water has been condensed, the hot solution is decanted from the precipitate formed on the container walls. The solvent is evaporated under reduced pressure and the residue is crystallized from toluene to yield 1,3-dithiane-2-carboxylic acid.

後処理

  1. additionthere are added 700 ml
  2. temperatureThe mixture is heated
  3. temperatureto reflux
  4. customcondensed
  5. customthe hot solution is decanted from the precipitate
  6. customformed on the container walls
  7. customThe solvent is evaporated under reduced pressure
  8. customthe residue is crystallized from toluene

出典と根拠

ORDレコード
ord-501c1721c44b41bdbdaa7cca61139b2e
出典データセット
uspto-grants-1976_03
特許番号
US03947469

関連ノート

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