StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Phosphoric Acid → 2,3,6,7-Tetramethoxyfluorenone

HRID 1586292
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1586292
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.P(=O)(O)(O)[OH:16].[CH3:20][O:21][C:22]1[CH:23]=[C:24]([C:30]2[CH:38]=[C:37]([O:39][CH3:40])[C:36]([O:41][CH3:42])=[CH:35][C:31]=2[C:32](O)=O)[CH:25]=[CH:26][C:27]=1[O:28][CH3:29]>O>[CH3:29][O:28][C:27]1[C:26](=[O:16])[C:25]2[C:24](=[CH:23][C:22]=1[O:21][CH3:20])[C:30]1[C:31](=[CH:35][C:36]([O:41][CH3:42])=[C:37]([O:39][CH3:40])[CH:38]=1)[CH:32]=2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1004Phosphoric AcidHCID 14812Phosphorus oxide (P4O10)HCID 154287532-(3,4-Dimethoxyphenyl)-4,5-dimethoxybenzoic acid

Produkt 1

HCID 675835612,3,6,7-Tetramethoxyfluorenone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Polyphosphoric acid which had been newly prepared from diphosphorus pentaoxide (50 g) and phosphoric acid (50 ml) was heated at 100° C. With stirring, 2-(3,4-dimethoxyphenyl)-4,5-dimethoxybenzoic acid (7.5 g) was added thereto as it is (in the crystal form) in several portions. After stirring at 100 to 120° C. for 2 hours, the reaction solution was poured into water (1.5 liter) and extracted with chloroform. The extract was washed with 2% aqueous sodium hydroxide solution, water and a saturated saline solution, then dried over sodium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent: chloroform) and recrystallized from ethyl acetate-n-hexane to give 5.0 g of 2,3,6,7-tetramethoxyfluorenone as an orange needle-like crystal.

Aufarbeitung

  1. stirringAfter stirring at 100 to 120° C. for 2 hours
  2. extractionextracted with chloroform
  3. washThe extract was washed with 2% aqueous sodium hydroxide solution, water
  4. dry with materiala saturated saline solution, then dried over sodium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was purified by silica gel column chromatography (eluent: chloroform)
  7. customrecrystallized from ethyl acetate-n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-dc981cb2ebcb44609214b1c8e3d97945
Quelldatensatz
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05942641

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion