Dichloromethane → HCID 59006363, Verbindung

HRID 1867605Notizen

Reaktionsgleichung

[OH-].COC(NS([N+](CC)(CC)CC)(=O)=O)=O.[NH2:17][C:18]([C:20]1[NH:21][C:22](=[O:38])[N:23]([CH:25]2[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27][CH2:26]2)[CH:24]=1)=O.ClCCl.C(=O)(O)[O-].[Na+]>ClC(Cl)C>[C:18]([C:20]1[NH:21][C:22](=[O:38])[N:23]([CH:25]2[CH2:26][CH2:27][N:28]([C:31]([O:33][C:34]([CH3:36])([CH3:35])[CH3:37])=[O:32])[CH2:29][CH2:30]2)[CH:24]=1)#[N:17]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

(Methoxycarbonylsulfamoyl)triethylammonium hydroxide, inner salt (179.7 mg, 0.754 mmol) was added to a solution of tert-butyl 4-[4-(aminocarbonyl)-2-oxo-2,3-dihydro-1H-imidazol-1-yl]piperidine-1-carboxylate (78 mg, 0.251 mmol) in dichloroethane (5 mL) and was heated to 50° C. After 1 h, the reaction was worked up with dichloromethane and saturated sodium bicarbonate. The organic extracts were washed with brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→5% methanol {1% ammonium hydroxide}/dichloromethane) gave the title compound (40 mg). MS 237.04 (M+1-tert butyl)

Aufarbeitung

washThe organic extracts were washed with brine
dry with materialdried over sodium sulfate
filtrationfiltered
concentrationconcentrated
customPurification by silica gel chromatography (100% dichloromethane→5% methanol {1% ammonium hydroxide}/dichloromethane)

Quellen und Nachweise

ORD-Eintrag: ord-05f908f0430b4cd795b481588415ca9f
Quelldatensatz: uspto-grants-2009_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07632832B2

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