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Hydrochloric Acid → 2,2-Bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane

HRID 1086324
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1086324
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([C:22]2[CH:27]=[CH:26][C:25]([OH:28])=[C:24]([N+:29]([O-:31])=[O:30])[CH:23]=2)([C:18]([F:21])([F:20])[F:19])[C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=1[N+:32]([O-:34])=[O:33].Cl>N1C=CC=CC=1>[S:2]([O:28][C:25]1[CH:26]=[CH:27][C:22]([C:13]([C:10]2[CH:11]=[CH:12][C:7]([O:6][S:2]([CH3:1])(=[O:4])=[O:3])=[C:8]([N+:32]([O-:34])=[O:33])[CH:9]=2)([C:18]([F:21])([F:19])[F:20])[C:14]([F:16])([F:15])[F:17])=[CH:23][C:24]=1[N+:29]([O-:31])=[O:30])([CH3:1])(=[O:4])=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 111336832,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

Produkt 1

HCID 142050422,2-Bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropaneAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

11.5 g (0.1 mol) of methanesulfonyl chloride are added dropwise, at a reaction temperature of 0-5° C., to a mixture of 21.3 g (0.05 mol) of 2,2-bis-(4-hydroxy-3-nitrophenyl)-hexafluoropropane and 100 ml of pyridine. Stirring is continued for 1 hour at 5° C. and overnight at room temperature. The reaction mixture is then acidified, first with dilute hydrochloric and then with half-concentrated hydrochloric acid; the precipitate which is deposited is filtered off with suction and washed with water until neutral. The crude product (29.3 g) is then recrystallized from toluene, resulting in 24.8 g of analytically pure 2,2-bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane to be isolated. Yield 85%; m.p. 119-121° C.

Aufarbeitung

  1. additionfirst with dilute hydrochloric
  2. filtrationthe precipitate which is deposited is filtered off with suction
  3. washwashed with water until neutral
  4. customThe crude product (29.3 g) is then recrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-367d7b325d334add9a422dc99a56328d
Quelldatensatz
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05028728

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