Triethylamine → HCID 73292226, Verbindung

HRID 1398036Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1398036
Cl.[NH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]([CH3:12])[CH3:11])[NH2:3].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20](=O)[CH2:21][C:22]([CH:24]2[CH2:29][C:28]([CH3:31])([CH3:30])[O:27][C:26]([CH3:33])([CH3:32])[CH2:25]2)=O)=[CH:16][CH:15]=1.C(N(CC)CC)C>CO.CCOC(C)=O>[Cl:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[N:2]([C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:10]([CH3:12])[CH3:11])[N:3]=[C:22]([CH:24]3[CH2:25][C:26]([CH3:33])([CH3:32])[O:27][C:28]([CH3:31])([CH3:30])[CH2:29]3)[CH:21]=2)=[CH:18][CH:19]=1

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 86722002HCID 86722002, VerbindungHCID 86722003HCID 86722003, Verbindung

Produkt 1

HCID 73292226HCID 73292226, VerbindungAusbeute 52,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of (2-hydrazino-phenyl)-dimethyl-amine hydrochloride (105 mg, 0.56 mmol), 1-(4-chloro-phenyl)-3-(2,2,6,6-tetramethyl-tetrahydro-pyran-4-yl)-propane-1,3-dione (162 mg, 0.50 mmol), and triethylamine (0.08 mL, 0.56 mmol), in 1.4 mL of methanol was stirred at RT for 8 hrs. The mixture was diluted with 20 mL of EtOAc and washed with saturated NaHCO3 (40 mL) and brine (40 mL). The organic layer was dried over Na2SO4, concentrated, and the residue purified by flash chromatography on silica gel to give 115 mg (47%) of the title compound as a white solid.

Aufarbeitung

  1. washwashed with saturated NaHCO3 (40 mL) and brine (40 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated
  4. customthe residue purified by flash chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-fd87fad3e1eb4df691254c69f8ee3219
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08901314B2

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