Triethylamine → HCID 11436590, Verbindung

HRID 343600

Reaktionsgleichung

Reaktionsgleichung von HRID 343600
[CH2:1]([NH:3][CH2:4][C:5]([OH:7])=O)[CH3:2].[CH3:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:10]=1[N:16]=[C:17]=[S:18].C(N(CC)CC)C>C(Cl)Cl>[CH3:15][C:11]1[CH:12]=[CH:13][CH:14]=[C:9]([CH3:8])[C:10]=1[N:16]1[C:5](=[O:7])[CH2:4][N:3]([CH2:1][CH3:2])[C:17]1=[S:18]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 879762,6-Xylyl isothiocyanateHCID 316542N-Ethylglycine

Produkt 1

HCID 11436590HCID 11436590, VerbindungAusbeute 18,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of N-ethyl glycine (9.2 g), 2,6-dimethylphenyl-isothiocyanate (8.2 g), triethylamine (10.1 g), and methylene chloride (150 mL) was heated at reflux for 3.5 hours. The mixture was evaporated to dryness. Purification was achieved through crystallization from ethanol. The title compound (2.3 g) was obtained as a white solid (2.3 g). m.p. 128°-131° C. Anal. Calcd. for. C13H16N2OS: C, 62.87; H, 6.49; N, 11.28. Found: C, 62.83; H, 6.50; N, 11.25. Mass spectrum (EI, M.+) m/z 248.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 3.5 hours
  3. customThe mixture was evaporated to dryness
  4. customPurification
  5. customwas achieved through crystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-497f500330044158bb46447d68ff46cf
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05861517

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