Triethylamine → HCID 18975625, Verbindung

HRID 2393327Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2393327
[CH2:1]([NH:3][CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH3:2].[CH3:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[C:11]=1[N:17]=[C:18]=[S:19].C(N(CC)CC)C>C(Cl)Cl>[CH3:16][C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([CH3:9])[C:11]=1[NH:17][C:18](=[S:19])[N:3]([CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH2:1][CH3:2]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 879762,6-Xylyl isothiocyanateHCID 12227201HCID 12227201, Verbindung

Produkt 1

HCID 18975625HCID 18975625, VerbindungAusbeute 39,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 3-ethylaminopropionic acid (19.8 g), 2,6-dimethylphenyl-isothiocyanate (16.3 g), triethylamine (20 g) and methylene chloride (200 mL) was heated at reflux for 3 hours. The cooled reaction mixture was extracted with 1N NaOH (150 mL). The aqueous layer was separated and acidified with 2N HCl. The solid formed was collected by filtration. Recrystallization from ethanol afforded the title compound (11 g) as a white solid, m.p. 115°-118° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customThe cooled reaction mixture
  4. extractionwas extracted with 1N NaOH (150 mL)
  5. customThe aqueous layer was separated
  6. customThe solid formed
  7. filtrationwas collected by filtration
  8. customRecrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-6625c77a72f04e8ea7be86a0aeae05ba
Quelldatensatz
uspto-grants-1998_09
Patentnummer
US05807864

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