HCID 117601197, Verbindung → HCID 117601899, Verbindung

HRID 1773744Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1773744
[CH3:1][C:2]1[C:6]([C:7]2[CH:8]=[C:9]([C:17]([O:19]C)=O)[C:10]3[NH:14][C:13](=[O:15])[NH:12][C:11]=3[CH:16]=2)=[C:5]([CH3:21])[O:4][N:3]=1.[CH:22]1([Mg]Cl)[CH2:26][CH2:25][CH2:24][CH2:23]1>C1COCC1>[CH:22]1([C:17]([C:9]2[C:10]3[NH:14][C:13](=[O:15])[NH:12][C:11]=3[CH:16]=[C:7]([C:6]3[C:2]([CH3:1])=[N:3][O:4][C:5]=3[CH3:21])[CH:8]=2)=[O:19])[CH2:26][CH2:25][CH2:24][CH2:23]1

Komponenten

4

Edukt 2

HCID 117601197HCID 117601197, VerbindungHCID 178478989HCID 178478989, Verbindung

Produkt 1

HCID 117601899HCID 117601899, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a mixture containing methyl 6-(3,5-dimethylisoxazol-4-yl)-2-oxo-2,3-dihydro-1H-benzo[d]imidazole-4-carboxylate (60 mg, 0.21 mmol, 1 equiv.) and THF (3 mL) is added cyclopentyl magnesium chloride (0.88 mL, 1.46 mmol, 7 equiv.) at 0° C. for 5 min. After completion, the reaction was quenched and extracted with EtOAc and washed with water, saturated NH4Cl. After drying with MgSO4, it was filtered and concentrated to dryness. Purification was carried out by reverse phase HPLC.

Aufarbeitung

  1. customAfter completion, the reaction was quenched
  2. extractionextracted with EtOAc
  3. washwashed with water, saturated NH4Cl
  4. dry with materialAfter drying with MgSO4, it
  5. filtrationwas filtered
  6. concentrationconcentrated to dryness
  7. customPurification

Quellen und Nachweise

ORD-Eintrag
ord-154bd48e69d64f63bb8e9af71b0db646
Quelldatensatz
uspto-grants-2016_02
Patentnummer
US09255089B2

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