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

Triethylamine → 7-Fluoro-1-methyl-4-oxo-1,4-dihydro-quinol-3-yl ethanesulphonate

HRID 358694
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 358694
[CH2:1]([S:3](Cl)(=[O:5])=[O:4])[CH3:2].[F:7][C:8]1[CH:17]=[C:16]2[C:11]([C:12](=[O:20])[C:13]([OH:19])=[CH:14][N:15]2[CH3:18])=[CH:10][CH:9]=1.C(N(CC)CC)C>ClCCl>[CH2:1]([S:3]([O:19][C:13]1[C:12](=[O:20])[C:11]2[C:16](=[CH:17][C:8]([F:7])=[CH:9][CH:10]=2)[N:15]([CH3:18])[CH:14]=1)(=[O:5])=[O:4])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chloride2×HCID 231281077-Fluoro-3-hydroxy-1-methyl-4quinolone

Produkt 1

HCID 540392937-Fluoro-1-methyl-4-oxo-1,4-dihydro-quinol-3-yl ethanesulphonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Ethanesulphonyl chloride (1.5 ml) was added to a stirred mixture of 7-fluoro-3-hydroxy-1-methyl-4quinolone (3.0 g), obtained as described in Example 3a-f, triethylamine (4.35 ml) and dry dichloromethane (100 ml) at ambient temperature and the resultant solution stirred for 5 minutes then kept at ambient temperature overnight. Further ethanesulphonyl chloride (0.2 ml) was added and the solution stirred at ambient temperature for 4 hours and then kept at this temperature for 3 days. The mixture was filtered and the filtrate was washed with water (2×150 ml). The dichloromethane solution was dried over magnesium sulphate and the solvent evaporated to give a residue which was crystallised from industrial methylated spirit (100 ml). The solid was triturated with diethyl ether (100 ml) and then water (500 ml) to give the novel compound 7-fluoro-1-methyl-4-oxo-1,4-dihydro-quinol-3-yl ethanesulphonate, m.p. 154°-156.5°.

Aufarbeitung

  1. customobtained
  2. waitkept at this temperature for 3 days
  3. filtrationThe mixture was filtered
  4. washthe filtrate was washed with water (2×150 ml)
  5. dry with materialThe dichloromethane solution was dried over magnesium sulphate
  6. customthe solvent evaporated
  7. customto give a residue which
  8. customwas crystallised from industrial methylated spirit (100 ml)
  9. customThe solid was triturated with diethyl ether (100 ml)

Quellen und Nachweise

ORD-Eintrag
ord-12525b913ada47238664b5f691b20e09
Quelldatensatz
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04997840

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion