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

6-Methylpyridine-2-carboxylic acid → HCID 44539828, Verbindung

HRID 1695793
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1695793
ClC(N(C)C)=C(C)C.[CH3:9][C:10]1[N:15]=[C:14]([C:16]([OH:18])=O)[CH:13]=[CH:12][CH:11]=1.[NH2:19][C:20]1[CH:28]=[C:27]([C:29]2[CH:30]=[C:31]([NH:36][S:37]([CH3:40])(=[O:39])=[O:38])[C:32]([Cl:35])=[N:33][CH:34]=2)[CH:26]=[C:25]2[C:21]=1[CH:22]=[N:23][N:24]2[CH3:41].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[Cl:35][C:32]1[N:33]=[CH:34][C:29]([C:27]2[CH:26]=[C:25]3[C:21]([CH:22]=[N:23][N:24]3[CH3:41])=[C:20]([NH:19][C:16]([C:14]3[CH:13]=[CH:12][CH:11]=[C:10]([CH3:9])[N:15]=3)=[O:18])[CH:28]=2)=[CH:30][C:31]=1[NH:36][S:37]([CH3:40])(=[O:39])=[O:38]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702826-Methylpyridine-2-carboxylic acidHCID 516892Sodium BicarbonateHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 86653304HCID 86653304, Verbindung

Produkt 1

HCID 44539828HCID 44539828, VerbindungAusbeute 6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel
4×

Versuchsvorschrift

1-Chloro-N,N,2-trimethyl-1-propen-1-amine (0.042 ml) was added to 6-methyl-2-pyridinecarboxylic acid (44 mg) in DCM (1 ml). The reaction was stirred at RT for 20 mins. N-[5-(4-Amino-1-methyl-1H-indazol-6-yl)-2-chloro-3-pyridinyl]methanesulfonamide (75 mg) in DCM (2 ml) was added and the reaction stirred for 30 mins. Approximately 4 ml saturated sodium bicarbonate (aq) was added followed by DCM (3 ml). The reaction was stirred vigorously. The DCM was passed through a hydrophobic frit then evaporated to dryness. The residue was dissolved in DMSO:methanol (1 ml, 1:1, v/v) and purified by MDAP (method E). The pure fraction was evaporated to dryness to give title compound (6 mg)

Aufarbeitung

  1. stirringthe reaction stirred for 30 mins
  2. stirringThe reaction was stirred vigorously
  3. customthen evaporated to dryness
  4. dissolutionThe residue was dissolved in DMSO
  5. custommethanol (1 ml, 1:1, v/v) and purified by MDAP (method E)
  6. customThe pure fraction was evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-89c4728f3106400da076ae4dcd23cb16
Quelldatensatz
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08163743B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion