Trifluoroacetic acid → HCID 20450402, Verbindung

HRID 358106Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358106
COC1C=CC(C[O:10][C:11]([CH2:13][C:14]([O:16][C:17]2[CH:18]=[C:19]([C:23]3[N:24]=[C:25]4[N:29]([CH:30]=3)[C:28]3[CH:31]=[CH:32][CH:33]=[CH:34][C:27]=3[S:26]4)[CH:20]=[CH:21][CH:22]=2)=[O:15])=[O:12])=CC=1.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O.C(O)C.[ClH:53]>ClCCl.O1CCCC1>[ClH:53].[C:11]([CH2:13][C:14]([O:16][C:17]1[CH:18]=[C:19]([C:23]2[N:24]=[C:25]3[N:29]([CH:30]=2)[C:28]2[CH:31]=[CH:32][CH:33]=[CH:34][C:27]=2[S:26]3)[CH:20]=[CH:21][CH:22]=1)=[O:15])([OH:12])=[O:10]

Komponenten

7

Edukt 4

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 13206728HCID 13206728, VerbindungHCID 21887872Ethanol hydrochloride

Produkt 1

HCID 20450402HCID 20450402, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In 5 ml of anhydrous dichloromethane was dissolved 1.146 g of 2-[m-(p-methoxyphenylmethoxycarbonylacetoxy)phenyl]imidazo[2,1-b]benzothiazole and after adding thereto 0.4 ml of anisole, the mixture was cooled with ice-water. Then, 5 ml of trifluoroacetic acid was added dropwise to the mixture and the resultant mixture was stirred for one hour. The reaction mixture thus formed was concentrated under reduced pressure and the oily product thus obtained was dissolved in 10 ml of anhydrous tetrahydrofuran. Then, while stirring the mixture under ice-cooling, 2 ml of 2N hydrogen chloride ethanol solution was added to the solution and white crystals thus precipitated were recovered by filtration to provide 911 mg of 2-(m-carboxyacetoxyphenyl)imidazo[2,1-b]benzothiazole hydrochloride.

Aufarbeitung

  1. additionafter adding
  2. customThe reaction mixture thus formed
  3. concentrationwas concentrated under reduced pressure
  4. customthe oily product thus obtained
  5. temperaturecooling
  6. customthus precipitated
  7. filtrationwere recovered by filtration

Quellen und Nachweise

ORD-Eintrag
ord-a6d31499b13c4a099b7626e686fd8ee8
Quelldatensatz
uspto-grants-1984_08
Patentnummer
US04464384

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