HCID 86655023, Verbindung → HCID 58333381, Verbindung

HRID 2066892Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2066892
[F:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:11])(=[O:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:17][CH2:16][C:15](=[N:18][O:19][CH:20]2[CH2:25][CH2:24][N:23]([C:26]#[N:27])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1.[OH:28][NH:29][C:30](=N)[CH:31]([CH3:33])[CH3:32]>C(OCC)(=O)C.[Cl-].[Cl-].[Zn+2]>[CH:31]([C:30]1[N:27]=[C:26]([N:23]2[CH2:24][CH2:25][CH:20]([O:19][N:18]=[C:15]3[CH2:16][CH2:17][N:12]([C:3]4[CH:4]=[CH:5][C:6]([S:8]([CH3:11])(=[O:9])=[O:10])=[CH:7][C:2]=4[F:1])[CH2:13][CH2:14]3)[CH2:21][CH2:22]2)[O:28][N:29]=1)([CH3:33])[CH3:32]

Komponenten

5

Edukt 2

HCID 86655023HCID 86655023, VerbindungHCID 178449908HCID 178449908, Verbindung

Produkt 1

HCID 58333381HCID 58333381, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

68b (35 mg, 0.066 mmol) and 68a (8 mg, 0.08 mmol) were combined in ethyl acetate (1 mL) and 1N ZnCl2 (80 μL, 0.08 mmol) was added dropwise. After 1 h, the solvent was evaporated. 1 mL of ethanol and 0.5 mL of concentrated HCl were added and the mixture was heated to reflux. The solvent was removed and the crude mixture was purified on preparative HPLC to give 68-1: LC-MS 480.2 (MH+), tR=5.57 (Method 5).

Aufarbeitung

  1. customthe solvent was evaporated
  2. addition1 mL of ethanol and 0.5 mL of concentrated HCl were added
  3. temperaturethe mixture was heated to reflux
  4. customThe solvent was removed
  5. customthe crude mixture was purified on preparative HPLC
  6. customto give 68-1

Quellen und Nachweise

ORD-Eintrag
ord-48cb117126574275b474e7ed042c68b9
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08293729B2

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