4-(4-Acetylaminophenyl)-1,2-Dihydro-1-Methyl-2-Ethylcarbamoyl-6-Methylthiophthalazine → HCID 9841541, Verbindung

HRID 2181610Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2181610
C([NH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([S:21][CH3:22])[CH:19]=3)[CH:14]([CH3:23])[N:13]([C:24](=[O:28])[NH:25][CH2:26][CH3:27])[N:12]=2)=[CH:7][CH:6]=1)(=O)C>CO.[OH-].[Na+].O>[NH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([S:21][CH3:22])[CH:19]=3)[CH:14]([CH3:23])[N:13]([C:24](=[O:28])[NH:25][CH2:26][CH3:27])[N:12]=2)=[CH:7][CH:6]=1

Komponenten

5

Edukt 1

HCID 129861734-(4-Acetylaminophenyl)-1,2-Dihydro-1-Methyl-2-Ethylcarbamoyl-6-Methylthiophthalazine

Produkt 1

HCID 9841541HCID 9841541, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

The solution of acetyl amide 9 in methanol and NaOH (2 N) was refluxing until there is no more starting material left monitored by TLC. The solution was diluted with water, and extracted with DCM three times. Removal of the solvent afforded the crude product, which was purified by using a silica gel column, gave the desired products 12 (Yield: 87%). 1HNMR (CDCl3): 7.45 (d, J=8.6 Hz, 2H), 7.35−7.25 (m, 4H), 6.78 (d, J=8.6 Hz, 2H), 6.53 (br, 1H), 5.60 (q, J=13.2 Hz, 1H), 3.42 (m, 2H), 2.40 (s, 3H), 1.22 (m, 6H).

Aufarbeitung

  1. waitleft
  2. extractionextracted with DCM three times
  3. customRemoval of the solvent
  4. customafforded the crude product, which
  5. customwas purified

Quellen und Nachweise

ORD-Eintrag
ord-62b2123549cd4420b123a55a9e50ab4e
Quelldatensatz
uspto-grants-2005_05
Patentnummer
US06894048B2

Notizen zur Reaktion

Wird geladen…