Ammonium Thioglycolate → HCID 131736786, Verbindung
Reaktionsgleichung
O=[As:2]O[As]=O.C([O-])(=O)CS.[NH4+].[CH2:12]([C:14]([CH2:19][SH:20])([CH2:17][SH:18])[CH2:15][SH:16])[CH3:13]>C(O)C>[CH2:12]([C:14]12[CH2:19][S:20][As:2]([S:18][CH2:17]1)[S:16][CH2:15]2)[CH3:13]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Arsenic trioxide (0.101 g, 0.506 mmol) was dissolved in ethanol (95%, 20 mL) and ammonium thioglycolate (827.2 μL of 5.5 M aqueous solution, 4.55 mmol) were stirred vigorously while heating to 50° C. After 60 minutes 4 (0.184 g, 1.01 mmol) was added, stirring continued for 20 minutes, cooled, and then filtered to remove insoluble material. The filtrate was taken to dryness, washed with water (2×15 mL), dissolved in dichloromethane (10 mL), dried over anhydrous magnesium sulfate, filtered, and taken to dryness to yield light yellow crystals. X-ray quality crystals were grown by slow evaporation from chloroform. Yield: 0.135 g, 50.3%. 1H NMR (CDCl3; 500 MHz) δ ppm: 0.89 (t, 3H, CH3), 1.39 (q, 2H, CH2) 2.94 (s, 6H, SCH2). 13C NMR (CDCl3 d6; 125.8 MHz) δ ppm: 8.17 (CH3), 31.29 (C), 31.65 (SCH2), 37.39 (CCH2). ESI-MS (m/z) 254.69 (254.93 calcd for [M+H]+ of [C6H11S3As]). Elemental Anal. calc'd (found) for C6H11S3As: C, 28.34 (31.42); H, 4.36 (4.70).
Aufarbeitung
- temperaturecooled
- filtrationfiltered
- customto remove insoluble material
- washwashed with water (2×15 mL)
- dissolutiondissolved in dichloromethane (10 mL)
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customto yield light yellow crystals
- customX-ray quality crystals were grown by slow evaporation from chloroform
Quellen und Nachweise
- ORD-Eintrag
- ord-0a9825509da942cc928865fcd19fcad1
- Quelldatensatz
- uspto-grants-2016_08
- Patentnummer
- US09427483B2
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