Methanethiol → HCID 19969723, Verbindung

HRID 974882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 974882
CC(C)([O-])C.[K+].[CH3:7][SH:8].[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[CH2:28]OS(C)(=O)=O)[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10]>CCO>[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[CH2:28][S:8][CH3:7])[CH2:18][CH2:17]1)=[O:15])([CH3:11])([CH3:10])[CH3:12]

Komponenten

5

Edukt 3

HCID 878MethanethiolHCID 19969748HCID 19969748, VerbindungHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 19969723HCID 19969723, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Potassium t-butoxide (159 mg, 1,42 mmol) in 15 mL of abs. EtOH was saturated with methyl mercaptan gas. To this mixture was added 1-t-butoxycarbonyl-4-(2-(methanesulfonyloxymethyl)phenyl)-piperazine (0.94 mmol, which was generated according to the procedure described in Step C of Example 9). The resulting mixture was refluxed for 50 min and concentrated. The residue was purified by preparative TLC (20% EtOAc in Hex) to give the title compound (157 mg).

Aufarbeitung

  1. temperatureThe resulting mixture was refluxed for 50 min
  2. concentrationconcentrated
  3. customThe residue was purified by preparative TLC (20% EtOAc in Hex)

Quellen und Nachweise

ORD-Eintrag
ord-da3aad95f0ec48ad9a75fbfe5c174f02
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05607936

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