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Chloroform → HCID 22137207, Verbindung

HRID 1827299
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1827299
[S:1]([Cl:5])(=[O:4])(=[O:3])O.C(Cl)Cl.[C:9]1([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:17][CH:16]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(Cl)(Cl)Cl>[Cl-].[Na+].O>[Cl:5][S:1]([C:12]1[CH:11]=[CH:10][C:9]([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:22]=[CH:23][C:24]([S:1]([Cl:5])(=[O:4])=[O:3])=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)=[CH:14][CH:13]=1)(=[O:4])=[O:3]
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Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 6344DichloromethaneHCID 7115p-TerphenylHCID 24638Chlorosulfonic acid3×

Produkt 1

HCID 22137207HCID 22137207, VerbindungAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 57417360
Sodium chloride; water
Lösungsmittel

Versuchsvorschrift

Under the nitrogen gas atmosphere, chloro sulfuric acid is diluted by adding chloro sulfuric acid (0.53 ml, 8 eq.) into methylene chloride (10 ml), and 1,1′:4′,1″-terphenyl (0.230 g, 1.0 mmol) is added gradually into a container in which diluted chloro sulfuric acid is contained keeping the temperature at 0° C., then stirred at the room temperature for 6 hours. The obtained reacted mixture is poured into brine, and deposited white insoluble is removed by suction filtration. Since the small amount of product is possible to be remained, the residue is washed well by methylene chloride. Then, this solution and the extracted solution are dried up using magnesium sulfate. Solvent is vaporized off under the vacuum condition, and the impurity is removed from the obtained crude product by isolating by a column chromatography (φ=50 mm, h=100 mm; CHCl3). Thus, 4,4″-dichlorosulfonyl1,1′:4′,1″-terphenyl (0.288 g, 0.67 mmol, 67%) is obtained as a colorless crystal (compound F).

Aufarbeitung

  1. customat 0° C.
  2. customThe obtained reacted mixture
  3. customdeposited white insoluble is removed by suction filtration
  4. washthe residue is washed well by methylene chloride
  5. customThen, this solution and the extracted solution are dried up
  6. customthe impurity is removed from the
  7. customobtained crude product

Quellen und Nachweise

ORD-Eintrag
ord-8e895a45e1394778ba92dc52382a4f9d
Quelldatensatz
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07053173B2

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