1,2-Dichloroethane → HCID 178441008, Verbindung

HRID 229995Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 229995
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([N:11]([CH2:24][C:25]2[CH:33]=[CH:32][C:28]([C:29]([OH:31])=O)=[CH:27][CH:26]=2)[C:12]2[N:16]([CH2:17][CH2:18][OH:19])[C:15]3[CH:20]=[CH:21][CH:22]=[CH:23][C:14]=3[N:13]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].O.[NH:35]1[C:39]([NH2:40])=[N:38][N:37]=[N:36]1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.CCN(C(C)C)C(C)C>CN(C=O)C>[C:1]([CH:5]1[CH2:6][CH2:7][CH:8]([N:11]([CH2:24][C:25]2[CH:26]=[CH:27][C:28]([C:29]([NH:40][C:39]3[NH:38][N:37]=[N:36][N:35]=3)=[O:31])=[CH:32][CH:33]=2)[C:12]2[N:16]([CH2:17][CH2:18][OH:19])[C:15]3[CH:20]=[CH:21][CH:22]=[CH:23][C:14]=3[N:13]=2)[CH2:9][CH2:10]1)([CH3:3])([CH3:4])[CH3:2]

Komponenten

7

Edukt 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 688378984-{[(4-Tert-butylcyclohexyl)(1-{2-hydroxyethyl}-1h-benzimidazol-2-yl)-amino]methyl}benzoic acidHCID 178509300HCID 178509300, Verbindung

Produkt 1

HCID 178441008HCID 178441008, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of the title compound of Example 10 Step B (0.04 mmol, 19 mg) 1H-tetraazol-5-amine monohydrate (0.13 mmol, 13 mg), HOBt (0.085 mmol, 13 mg) and EDC (0.17 mmol, 33 mg) in 0.5 mL of DMF was added DIEA (0.21 mmol, 36 μL). The reaction mixture was allowed to stand at ambient temperature overnight, then concentrated under reduced pressure. The residue was taken up in ca. 2:1 dioxane/H2O and acidified with TFA, then purified by reverse-phase chromatography (Condition B). The product was lyophilized, affording the title compound as a white solid. MS (ESI): m/z 517 (M+H). HPLC A: 1.81 min.

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. custompurified by reverse-phase chromatography (Condition B)

Quellen und Nachweise

ORD-Eintrag
ord-131c5d630577494eb04e6d088c9a28db
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563815B2

Notizen zur Reaktion

Wird geladen…