Ethanolamine → HCID 49785857, Verbindung

HRID 2389858

Reaktionsgleichung

Reaktionsgleichung von HRID 2389858
[Cl:1][C:2]1[C:11]2[C:12]3[C:17]([NH:18][C:10]=2[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1)=[CH:16][CH:15]=[CH:14][CH:13]=3.[NH:19]1C2C(=CC=CC=2)[C:22](=[O:23])[C:20]1=O.NCCO.CO>C(OCCO)C>[ClH:1].[CH:8]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:9]=1[C:10]1[NH:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]=1[C:2]([NH:19][CH2:20][CH2:22][OH:23])=[N:3]2

Komponenten

6

Edukt 4

HCID 700EthanolamineHCID 887MethanolHCID 7054IsatinHCID 54103076-Chloro-11H-indolo[3,2-c]quinoline

Produkt 1

HCID 49785857HCID 49785857, VerbindungAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8076Glycol monoethyl etherLösungsmittel

Versuchsvorschrift

A mixture of compound 4a as obtained from the above Synthesis Ex. 1 (0.50 g, 2 mmol) and 2-aminoethanol (0.24 g, 4 mmol) in 2-ethoxyethanol (20 mL) was heated at 140-150° C. for 48 hrs (by TLC monitoring). After cooling, the reaction mixture was evaporated in vacuo to give a residue, which was treated with MeOH (30 mL) to result in precipitation. The resultant precipitate was collected by filtration and recrystallized with MeOH to give the title compound 7d as a white powder (0.38 g, 61% yield).

Aufarbeitung

  1. customas obtained from the above Synthesis Ex
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated in vacuo
  4. customto give a residue, which
  5. customto result in precipitation
  6. filtrationThe resultant precipitate was collected by filtration
  7. customrecrystallized with MeOH

Quellen und Nachweise

ORD-Eintrag
ord-60acdee8c7cb47a29c3076f9021f1857
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08273760B2

Verknüpfte Notizen

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