Chloroacetonitrile → HCID 19837048, Verbindung

HRID 476876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 476876
[CH3:1][C:2]1[CH:3]=[C:4]2[C:11](=[CH:12][CH:13]=1)[C:7]([CH2:8][CH2:9][NH2:10])=[CH:6][NH:5]2.Cl[CH2:15][C:16]#[N:17]>O1CCCC1.C(Cl)Cl>[CH3:1][C:2]1[CH:3]=[C:4]2[C:11]([C:7]([CH2:8][CH2:9][NH:10][CH2:15][C:16]#[N:17])=[CH:6][NH:5]2)=[CH:12][CH:13]=1

Komponenten

5

Edukt 2

HCID 7856ChloroacetonitrileHCID 1900062-(6-Methyl-1H-indol-3-yl)ethan-1-amine

Produkt 1

HCID 19837048HCID 19837048, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

17 g of 6-methyltryptamine were dissolved at 40° C. under inert atmosphere in 500 ml of tetrahydrofuran, and the solution was allowed to return to ambient temperature. 14.6 ml of 1,5-diaza[5,4,0]undec-5-ene were added followed by 6.2 ml of chloroacetonitrile and stirring for 15 hours. The solvent was eliminated under reduced pressure and the residue was taken up in 250 ml of methylene chloride, washed with water, dried and concentrated to dryness. The 25 g of crude product was purified by chromatography on silica (eluent: methylene chloride-ethyl acetate 3-7) to obtain 13.2 g of the expected product melting at 92° C.

Aufarbeitung

  1. customto return to ambient temperature
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated to dryness
  5. customThe 25 g of crude product was purified by chromatography on silica (eluent: methylene chloride-ethyl acetate 3-7)

Quellen und Nachweise

ORD-Eintrag
ord-18c2620c8e904afd9387c033a505751a
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04886802

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