p-Toluenesulfonic acid → HCID 67172923, Verbindung

HRID 406963

Reaktionsgleichung

Reaktionsgleichung von HRID 406963
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH3:7])[C:4]([OH:6])=[O:5].C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]([C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)(OC)OC)=[CH:24][CH:23]=1>C1(C)C=CC=CC=1>[Cl:21][C:22]1[CH:23]=[CH:24][C:25]([C:28]2([C:33]3[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=3)[O:9][CH2:8][C:3]([CH3:7])([C:4]([OH:6])=[O:5])[CH2:2][O:1]2)=[CH:26][CH:27]=1

Komponenten

5

Edukt 3

HCID 6101p-Toluenesulfonic acidHCID 78501Dimethylolpropionic acidHCID 11652307Benzene, 1,1'-(dimethoxymethylene)bis[4-chloro-

Produkt 1

HCID 67172923HCID 67172923, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

In a round bottom flask, (0.9 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and (9.8 mg) p-toluene sulfonic acid and 2 ml toluene was taken. The reaction mixture was stirred at room temperature and subsequently 2 g (1 equiv) bis-(4-chlorophenyl)-dimethoxymethane [IIa4] diluted with 5 ml toluene was added through droping funnel. The reaction mixture was heated at reflux temperature and the water was removed azeotropically under Dean Stark. Continuous removal and addition of toluene was done up to 2 hrs. Then the reaction mixture was cooled at room temperature to obtain off white solid. It was filtered and washed with toluene and then water.

Aufarbeitung

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux temperature
  4. customthe water was removed azeotropically under Dean Stark
  5. customContinuous removal and addition of toluene
  6. temperatureThen the reaction mixture was cooled at room temperature
  7. customto obtain off white solid
  8. filtrationIt was filtered
  9. washwashed with toluene

Quellen und Nachweise

ORD-Eintrag
ord-adb7d08ad9a84ddea06d239a776d91c8
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08754207B2

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