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Water → HCID 60064118, Verbindung

HRID 412601
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 412601
[C:1]([N:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][C:8]([SH:14])=[CH:9][CH:10]=2)[CH2:5]1)(=[O:3])[CH3:2].[H-].[Na+].[C:17]([O:21][C:22]([N:24]1[CH2:29][CH2:28][C:27]([C:33]([O:35][CH2:36][CH3:37])=[O:34])([CH2:30][CH2:31]I)[CH2:26][CH2:25]1)=[O:23])([CH3:20])([CH3:19])[CH3:18].O>CN(C)C=O>[C:17]([O:21][C:22]([N:24]1[CH2:29][CH2:28][C:27]([CH2:30][CH2:31][S:14][C:8]2[CH:7]=[C:6]3[C:11]([CH2:12][CH2:13][N:4]([C:1](=[O:3])[CH3:2])[CH2:5]3)=[CH:10][CH:9]=2)([C:33]([O:35][CH2:36][CH3:37])=[O:34])[CH2:26][CH2:25]1)=[O:23])([CH3:20])([CH3:19])[CH3:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 24758Sodium hydrideHCID 126069591-(3,4-Dihydro-7-mercapto-2(1H)-isoquinolinyl)ethanoneHCID 600641644-Ethoxycarbonyl-4-(2-iodoethyl)piperidine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 60064118HCID 60064118, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Crude crystals (1.26 g) of 2-acetyl-1,2,3,4-tetrahydroisoquinoline-7-thiol were dissolved in dimethylformamide (15 ml) and thereto were added 60% sodium hydride (243 mg) and 4-ethoxycarbonyl-4-(2-iodoethyl)piperidine-1-carboxylic acid tert-butyl ester (1 g), and the mixture was stirred at 70° C. for 1 hour. After completion of the reaction, water was added and the mixture was extracted with ethyl acetate and washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:7) and dried under reduced pressure to give the title compound (535 mg).

Aufarbeitung

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:7)
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-576a0026cdd141b4bfc63f68074159fc
Quelldatensatz
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06562828B1

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