1,2-Dichloroethane → HCID 58333608, Verbindung

HRID 2066848Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2066848
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28]([OH:30])=O)=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].[CH3:32][NH:33][CH3:34].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:8][CH2:9][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](=[O:30])[N:33]([CH3:34])[CH3:32])=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:11][CH2:12]1)=[O:6])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 111,2-DichloroethaneHCID 674DimethylamineHCID 757711-HydroxybenzotriazoleHCID 58333593HCID 58333593, Verbindung

Produkt 1

HCID 58333608HCID 58333608, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

9-1 (30 mg, 0.071 mmol), dimethylamine (0.1 mmol) and HOBT (0.2 mmol) were combined in DCM (1 mL) and stirred at room temperature for 10 minutes. EDC(0.2 mmol) was added and the mixture was stirred for 18 h. The solution was washed with 2 mL of aqueous NaHCO3, concentrated, taken up with 1 mL of methanol and purified on preparative HPLC to give 29-1: LC-MS 467.4 (MH).

Aufarbeitung

  1. stirringthe mixture was stirred for 18 h
  2. washThe solution was washed with 2 mL of aqueous NaHCO3
  3. concentrationconcentrated
  4. custompurified on preparative HPLC
  5. customto give 29-1

Quellen und Nachweise

ORD-Eintrag
ord-d5579f41056b452ebc62ec00f75f7468
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08293729B2

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