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Hydrochloric Acid → Bis(2-methyl-3-phenyl-1H-inden-7-yl) sulfide

HRID 2357868
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2357868
[CH3:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[S:11][C:12]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:13]=2[CH2:14][CH:15]([CH3:22])[C:16]3=O)[C:3]1=O.[C:24]1([Mg]Br)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[Mg].Br[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.Cl>CCOCC.O>[CH3:1][C:2]1[CH2:10][C:9]2[C:4]([C:3]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[CH:5][CH:6]=[CH:7][C:8]=2[S:11][C:12]1[CH:20]=[CH:19][CH:18]=[C:17]2[C:13]=1[CH2:14][C:15]([CH3:22])=[C:16]2[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 7961BromobenzeneHCID 5462224MagnesiumHCID 588977942-methyl-4-[(2-methyl-1-oxo-2,3-dihydro-1H-inden-4-yl)sulfanyl]-1-indanoneHCID 178418255HCID 178418255, Verbindung

Produkt 1

HCID 58897800Bis(2-methyl-3-phenyl-1H-inden-7-yl) sulfide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Under an argon atmosphere, to a solution of 3.20 g (9.93 mmol) of 2-methyl-4-[(2-methyl-1-oxo-2,3-dihydro-1H-inden-4-yl)sulfanyl]-1-indanone in 20 ml of ether, a solution of PhMgBr in ether [obtained from 0.73 g (30.0 mmol) of magnesium turnings, 4.77 g (30.4 mmol) of bromobenzene, and 30 ml of ether] was added dropwise with vigorous stirring at 0° C. This mixture was stirred overnight and then added to 50 ml of water. Then, to this mixture 12 M HCl (to pH 1) was added. The organic layer was separated; and the aqueous layer was extracted with 3×20 ml of dichloromethane. The combined extract was evaporated, and a mixture of the residue and 0.5 g para-toluenesulfonic acid in 150 ml benzene was refluxed for 1 hour. The resulting mixture was washed with 50 ml of saturated aqueous NaHCO3. The organic layer was separated, dried over Na2SO4, and evaporated to dryness. The product was isolated by flash chromatography on Silica Gel 60 (40-63 μm, d 35 mm, l 300 mm, eluant: hexanes-CH2Cl2=1:2, vol.). Yield, 2.20 g (50%) of a yellowish solid.

Aufarbeitung

  1. stirringThis mixture was stirred overnight
  2. customThe organic layer was separated
  3. extractionand the aqueous layer was extracted with 3×20 ml of dichloromethane
  4. extractionThe combined extract
  5. customwas evaporated
  6. additiona mixture of the residue and 0.5 g para-toluenesulfonic acid in 150 ml benzene
  7. temperaturewas refluxed for 1 hour
  8. washThe resulting mixture was washed with 50 ml of saturated aqueous NaHCO3
  9. customThe organic layer was separated
  10. dry with materialdried over Na2SO4
  11. customevaporated to dryness
  12. customThe product was isolated by flash chromatography on Silica Gel 60 (40-63 μm, d 35 mm, l 300 mm, eluant: hexanes-CH2Cl2=1:2, vol.)
  13. customYield

Quellen und Nachweise

ORD-Eintrag
ord-d44296ed4d704db3a0c32e34abadeead
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07763562B2

Notizen zur Reaktion

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