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Potassium Carbonate → HCID 14720317, Verbindung

HRID 2351986
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2351986
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([NH:9][CH2:10][C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)[CH:6]=[CH:7][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:25][S:26](Cl)(=[O:28])=[O:27].C(=O)(O)[O-].[Na+]>ClCCl>[N:13]1[CH:14]=[CH:15][CH:16]=[C:11]([CH2:10][N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:17])[F:18])[CH:4]=2)[S:26]([CH3:25])(=[O:28])=[O:27])[CH:12]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chloride2×HCID 516892Sodium BicarbonateHCID 147203163-(3-Trifluoromethylphenylaminomethyl)pyridine

Produkt 1

HCID 14720317HCID 14720317, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel

Versuchsvorschrift

A 3.8 g. portion of 3-(3-trifluoromethylphenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane and to it was added 2.7 g. of potassium carbonate and 1.6 ml. of methanesulfonyl chloride. The mixture was stirred at ambient temperature overnight, and at a gentle reflux for another day. Another 1.6 ml. of methanesulfonyl chloride was added, and the mixture was stirred under reflux for 3 days more. It was then cooled, and diluted with 20 ml. of aqueous sodium bicarbonate. The organic phase was separated, washed with water, dried and evaporated under vacuum. The residue was triturated with diethyl ether and petroleum ether, and dried to give 4.7 g. of the desired product, m.p. 106°-110°.

Aufarbeitung

  1. temperatureat a gentle reflux for another day
  2. stirringthe mixture was stirred
  3. temperatureunder reflux for 3 days more
  4. temperatureIt was then cooled
  5. additiondiluted with 20 ml
  6. customThe organic phase was separated
  7. washwashed with water
  8. customdried
  9. customevaporated under vacuum
  10. customThe residue was triturated with diethyl ether and petroleum ether
  11. customdried
  12. customto give 4.7 g

Quellen und Nachweise

ORD-Eintrag
ord-79786a6b06ae4ec0866514e6ae50fdba
Quelldatensatz
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04874775

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