Triethylamine → HCID 13534703, Verbindung

HRID 4361

Reaktionsgleichung

Reaktionsgleichung von HRID 4361
Cl.[NH2:2][N:3]1[CH2:8][CH:7]=[CH:6][CH2:5][CH2:4]1.C(N(CC)CC)C.[F:16][C:17]1[CH:18]=[C:19]([N:23]=[C:24]=[O:25])[CH:20]=[CH:21][CH:22]=1>C(Cl)Cl>[F:16][C:17]1[CH:18]=[C:19]([NH:23][C:24]([NH:2][N:3]2[CH2:4][CH:5]=[CH:6][CH2:7][CH2:8]2)=[O:25])[CH:20]=[CH:21][CH:22]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 1230643-Fluorophenyl isocyanateHCID 193760471,2,3,6-Tetrahydropyridin-1-amine hydrochloride

Produkt 1

HCID 13534703HCID 13534703, VerbindungAusbeute 60,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.012 g) in dry methylene chloride (40 ml) was added a solution of 3-fluorophenyl isocyanate (1.37 g) in dry methylene chloride under ice-bath cooling. After stirring for one hour, the reaction mixture was evaporated to dryness. The residue was extracted with ethyl acetate (100 ml). The extract was washed with water, evaporated to dryness and recystallized from ethyl acetate to give N-[[(3-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine (1.43 g). mp: 136.5°-138.5° C.

Aufarbeitung

  1. temperaturecooling
  2. customthe reaction mixture was evaporated to dryness
  3. extractionThe residue was extracted with ethyl acetate (100 ml)
  4. washThe extract was washed with water
  5. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-15946ac52f84452daf9d7ce6d8f8fe10
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04725608

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