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

Methyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate → HCID 15029431, Verbindung

HRID 1588455
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1588455
C[Al](C)C.[N:5]1([S:10]([CH:13]([S:15]([NH2:18])(=[O:17])=[O:16])[CH3:14])(=[O:12])=[O:11])[CH2:9][CH2:8][CH2:7][CH2:6]1.[CH3:19][O:20][C:21]1[N:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29](=O)[O:30]C)[N:22]=1>C1(C)C=CC=CC=1.ClCCl>[CH3:19][O:20][C:21]1[N:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29](=[O:30])[NH:18][S:15]([CH:13]([S:10]([N:5]2[CH2:9][CH2:8][CH2:7][CH2:6]2)(=[O:11])=[O:12])[CH3:14])(=[O:17])=[O:16])[N:22]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 14404501Methyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamateHCID 15029429HCID 15029429, VerbindungHCID 16682925Trimethylaluminum

Produkt 1

HCID 15029431HCID 15029431, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittel
HCID 6344
Dichloromethane
Lösungsmittel
2×

Versuchsvorschrift

9 ml (0.018 mol) of a 2M solution of trimethylaluminum in toluene are added dropwise at room temperature to 3.6 g (0.015 mol) of 1-pyrrolidinosulfonylethanesulfonamide (Example 1a) in 150 ml of dichloromethane. When the evolution of gas has ceased, 3.6 g (0.018 mol) of methyl 4-methoxy-6-methyl-1,3,5-triazin-2-ylcarbamate in 30 ml of dichloromethane are added dropwise, and the resulting solution is refluxed for 24 hours. It is cooled and poured into 150 ml of ice-cold 1N hydrochloric acid. The organic phase is separated off, and the water phase is extracted twice with dichloromethane. The organic phase is dried and evaporated. After the crude product has been triturated with diethyl ether, 2.9 g (47% of theory) of 3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1-(1-pyrrolidinosulfonylethylsulfonyl)urea of melting point 136°-137° C. are obtained.

Aufarbeitung

  1. temperaturethe resulting solution is refluxed for 24 hours
  2. temperatureIt is cooled
  3. customThe organic phase is separated off
  4. extractionthe water phase is extracted twice with dichloromethane
  5. customThe organic phase is dried
  6. customevaporated
  7. customAfter the crude product has been triturated with diethyl ether, 2.9 g (47% of theory) of 3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1-(1-pyrrolidinosulfonylethylsulfonyl)urea of melting point 136°-137° C.
  8. customare obtained

Quellen und Nachweise

ORD-Eintrag
ord-f0b572fbc6fd44e68538dda552923942
Quelldatensatz
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05223017

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion