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

1-Hydroxybenzotriazole → HCID 68797990, Verbindung

HRID 1375386
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1375386
[Cl:1][C:2]1[CH:30]=[C:29]([N:31]2[CH:35]=[CH:34][C:33]([CH3:36])=[N:32]2)[CH:28]=[CH:27][C:3]=1[C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2/[C:10](=[CH:17]/[C:18]([NH:20][CH2:21][C:22](O)=[O:23])=[O:19])/[C:9]([F:26])([F:25])[CH2:8][CH2:7]1)=[O:5].C1C=CC2N(O)N=[N:43][C:41]=2C=1.CCN=C=NCCCN(C)C.Cl.CN.C1COCC1.C([O-])(O)=O.[Na+]>C1COCC1>[Cl:1][C:2]1[CH:30]=[C:29]([N:31]2[CH:35]=[CH:34][C:33]([CH3:36])=[N:32]2)[CH:28]=[CH:27][C:3]=1[C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2/[C:10](=[CH:17]/[C:18]([NH:20][CH2:21][C:22]([NH:43][CH3:41])=[O:23])=[O:19])/[C:9]([F:26])([F:25])[CH2:8][CH2:7]1)=[O:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 44520870HCID 44520870, VerbindungHCID 66615946Methylamine tetrahydrofuran

Produkt 1

HCID 68797990
HCID 68797990, Verbindung
Ausbeute 19,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 258 mg of the compound of Example 10, 71 mg of HOBt and 101 mg of EDCI.HCl in 5 ml of THF, and 0.5 ml of 2.0 M methylamine-THF solution were added, and the mixture was stirred at room temperature overnight. The reaction solution was mixed with saturated NaHCO3 aq. and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The crude product obtained by evaporation of the solvent was purified by silica gel column chromatography (chloroform-MeOH (30:1)). The residue obtained by concentration under reduced pressure was crystallized from a 2-propanol-hexane solvent mixture to obtain 51 mg of (2Z)-2-{1-[2-chloro-4-(3-methyl-1H-pyrazol-1-yl)benzoyl]-4,4-difluoro-1,2,3,4-tetrahydro-5H-1-benzazepin-5-ylidene}-N-[2-(methylamino)-2-oxoethyl]acetamide.

Aufarbeitung

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe crude product obtained by evaporation of the solvent
  4. customwas purified by silica gel column chromatography (chloroform-MeOH (30:1))
  5. customThe residue obtained by concentration under reduced pressure
  6. customwas crystallized from a 2-propanol-hexane solvent mixture

Quellen und Nachweise

ORD-Eintrag
ord-6dccc9f7f5be40ab8c00b2c509096445
Quelldatensatz
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07169772B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion