Hydrazine → HCID 58550577, Verbindung

HRID 388859Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 388859
[O:1]=[C:2]1[N:10]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C@@:3]21[CH2:34][C:21]1=[N:22][C:23]3[CH:24]=[CH:25][C:26]([C:30](OC)=[O:31])=[CH:27][C:28]=3[CH:29]=[C:20]1[CH2:19]2.[NH2:35][NH2:36]>CO>[O:1]=[C:2]1[N:10]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:17])([CH3:16])[CH3:18])[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C@@:3]21[CH2:34][C:21]1=[N:22][C:23]3[CH:24]=[CH:25][C:26]([C:30]([NH:35][NH2:36])=[O:31])=[CH:27][C:28]=3[CH:29]=[C:20]1[CH2:19]2

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 58550631HCID 58550631, Verbindung

Produkt 1

HCID 58550577HCID 58550577, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a solution of methyl (2S)-2′-oxo-1′-{[2-(trimethylsilyl)ethoxy]methyl}-1,1′,2′,3-tetrahydrospiro[cyclopenta[b]quinoline-2,3′-pyrrolo[2,3-b]pyridine]-7-carboxylate from Step G (317 mg, 0.667 mmol) in MeOH (1 mL) was added hydrazine (1.0 mL, 32 mmol). The reaction was sealed and then heated to 70° C. for 18 hours. After cooling to ambient temperature, the bulk of the solvent was removed in vacuo. The residue was diluted with DCM (50 mL) and water (20 mL). The organics were then successively washed with water, half-saturated brine and brine before being dried over sodium sulfate. The organics were then filtered, concentrated in vacuo to give the title compound. MS: m/z=476 (M+1).

Aufarbeitung

  1. customThe reaction was sealed
  2. temperatureAfter cooling to ambient temperature
  3. customthe bulk of the solvent was removed in vacuo
  4. additionThe residue was diluted with DCM (50 mL) and water (20 mL)
  5. washThe organics were then successively washed with water, half-saturated brine and brine
  6. dry with materialbefore being dried over sodium sulfate
  7. filtrationThe organics were then filtered
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e74dd9bb188e426bb31d49141d084c9f
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08377955B2

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