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

HRID 268322

반응식

HRID 268322 반응식
[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]

참가 물질

5

반응물 4

HCID 241BenzeneHCID 962Water2회HCID 6101p-Toluenesulfonic acidHCID 80131,3-Propanedithiol

생성물 1

HCID 3037051,3-Dithiane-2-carboxylic acid

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-501c1721c44b41bdbdaa7cca61139b2e
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947469

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