Hydrazine hydrate (1:1) → HCID 178452593, Verbindung

HRID 1509153Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1509153
[C:1]([O:5][C:6](=[O:35])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:20][C:21]4[NH:26][C:25](=S)[CH2:24][O:23][C:22]=4[N:28]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].O.[NH2:37][NH2:38]>C1COCC1>[C:1]([O:5][C:6](=[O:35])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:20][C:21]4[NH:26]/[C:25](=[N:37]/[NH2:38])/[CH2:24][O:23][C:22]=4[N:28]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 86683631Tert-butyl (1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate

Produkt 1

HCID 178452593HCID 178452593, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl(1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate (2 g, 2.05 mmol) in THF (350 mL) was added hydrazine monohydrate (645 μl, 20.51 mmol) to give a yellow solution. The resulting mixture was stirred at room temperature for 2 hours. The mixture was filtered to remove insoluble black particles and concentrated to dryness under reduced pressure. The resulting yellow solid was used directly in the following step as crude without any further purification. LCMS (Method D): RT=1.04 min, M+1=486.

Aufarbeitung

  1. customto give a yellow solution
  2. filtrationThe mixture was filtered
  3. customto remove insoluble black particles
  4. concentrationconcentrated to dryness under reduced pressure
  5. customThe resulting yellow solid was used directly in the following step as crude without any further purification

Quellen und Nachweise

ORD-Eintrag
ord-5ae326018fa045cf9701e07ac78652bf
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09221838B2

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