Hydrochloric Acid → HCID 178477340, Verbindung

HRID 2300826

Reaktionsgleichung

Reaktionsgleichung von HRID 2300826
[C:1]([O:5]CC)(=O)[CH2:2][CH3:3].C[O-].[Na+].[CH:11](OCC)=O.[CH2:16]([S:18][C:19](=[NH:21])[NH2:20])[CH3:17].Cl>CN(C=O)C.CO>[CH2:16]([S:18][C:19]1[N:20]=[C:1]([OH:5])[C:2]([CH3:3])=[CH:11][N:21]=1)[CH3:17]

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 5139S-EthylisothioureaHCID 7749Ethyl PropionateHCID 8025Ethyl formateHCID 10942334Sodium Methoxide

Produkt 1

HCID 178477340HCID 178477340, VerbindungAusbeute 13,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of ethyl propionate (1.2 mL, 10 mmol) in DMF (1 mL) was added sodium methoxide (740 mg, 13 mmol), and to this was added ethyl formate (560 μL, 6.7 mmol) very slowly over 1 h period. The reaction mixture was stirred for 30 min then 2-ethyl-2-thiopseudourea (1.3 g, 6.7 mmol) in methanol (2.5 mL) was added at once. The mixture was heated and maintained at reflux for 2 h, cooled to room temperature and acidified to pH 6 with concentrated HCl. The resulting slurry was kept in ice bath for 30 minutes. The solid was collected and was rinsed with methanol. The solid was dried under vacuum to give 154 mg of the title compound. Mass spectrum 171.1 (CI, M+1).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperaturemaintained
  3. temperatureat reflux for 2 h
  4. customfor 30 minutes
  5. customThe solid was collected
  6. washwas rinsed with methanol
  7. customThe solid was dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-c01007e9015e4fbebc490d43cfe309be
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06498165B1

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