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Sodium Carbonate → HCID 178503549, Verbindung

HRID 2353640
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2353640
S(O)(O)(=O)=O.[CH3:6][S:7][C:8](=[NH:10])[NH2:9].[Cl:11][CH2:12][C:13](=O)[CH2:14][C:15](OCC)=[O:16].C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:11][CH2:12][C:13]1[N:9]=[C:8]([S:7][CH3:6])[N:10]=[C:15]([OH:16])[CH:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 69484Ethyl 4-chloroacetoacetateHCID 752702-Methyl-2-thiopseudourea sulfate

Produkt 1

HCID 178503549HCID 178503549, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

S-Methyl-2-thiopseudourea sulphate (20 g, 71.85 mmol), ethyl 4-chloroacetoacetate (10.755 ml, 79.04 mmol) and sodium carbonate (13.925 g, 107.78 mmol) were dissolved in water (100 ml) and stirred at room temperature overnight. The reaction was monitored by TLC, and once complete, the reaction precipitate was collected and the supernatant was neutralised with 6N hydrochloric acid to yield more reaction precipitate which was also collected. The accumulated precipitate was then washed with water (×3) and an off-white solid was obtained. This was dried in vacuo at 60° C. for 48 hours to yield the desired compound as a pale yellow/white solid, 43.2 g.

Aufarbeitung

  1. customonce complete, the reaction precipitate was collected
  2. customto yield more
  3. customreaction precipitate which
  4. customwas also collected
  5. washThe accumulated precipitate was then washed with water (×3)
  6. customan off-white solid was obtained
  7. customThis was dried in vacuo at 60° C. for 48 hours

Quellen und Nachweise

ORD-Eintrag
ord-2115342f0cbd4b5a95e8a6005d9214d3
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07750003B2

Notizen zur Reaktion

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