Sodium Carbonate → HCID 70193430, Verbindung

HRID 2186428Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2186428
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:8]=[CH:9][N:10]([CH:12]([CH3:16])[CH2:13][CH:14]=O)[CH:11]=2)[CH:2]=1.[NH:17]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[NH2:18].C(=O)([O-])[O-].[Na+].[Na+]>CC(O)=O.O.CCOC(C)=O>[CH3:23][C:22]([O:21][C:19]([NH:17][NH:18][CH2:14][CH2:13][C@H:12]([N:10]1[CH:11]=[C:7]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[N:8]=[CH:9]1)[CH3:16])=[O:20])([CH3:25])[CH3:24]

Komponenten

7

Edukt 3

HCID 10340Sodium CarbonateHCID 70091tert-Butyl carbazateHCID 18759767β-Methyl-4-(3-pyridinyl)-1H-imidazole-1-propanal

Produkt 1

HCID 70193430HCID 70193430, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

(R/S)-3-(4-pyridin-3-yl-imidazol-1-yl)-butan-1-al (11) (1 mmol) is dissolved in 10 mL HOAc and t-butyl hydrazinecarboxylate (1.1 mmol) is added. After 1 h, NaHB(OAc)3 (5 mmol) is added at 25° C. After 2 h, the reaction is poured into sodium carbonate in water and EtOAc. The water layer is removed, the organics are washed with brine, and dried over sodium sulfate. The solvent is removed in vacuo to leave the product (32).

Aufarbeitung

  1. waitAfter 2 h
  2. customThe water layer is removed
  3. washthe organics are washed with brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent is removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ecf2ad3b1cd74d89a09ecf67779636c5
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06403776B1

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