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Diethyl Ether → HCID 13020484, Verbindung

HRID 2198520
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2198520
Cl.[CH:2]1([CH2:15][C:16]([O:18]CC)=O)[C:7]2[NH:8][C:9]3[C:14]([C:6]=2[CH2:5][CH2:4][NH:3]1)=[CH:13][CH:12]=[CH:11][CH:10]=3.[O-:21][C:22]#[N:23].[Na+].[CH3:25]COCC>O>[CH3:25][N:23]1[C:16](=[O:18])[CH2:15][CH:2]2[C:7]3[NH:8][C:9]4[C:14]([C:6]=3[CH2:5][CH2:4][N:3]2[C:22]1=[O:21])=[CH:13][CH:12]=[CH:11][CH:10]=4
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 3283Diethyl Ether2×HCID 517096Sodium CyanateHCID 20519381Ethyl (2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)acetate--hydrogen chloride (1/1)

Produkt 1

HCID 13020484HCID 13020484, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Versuchsvorschrift

26 g (0.088 mol) of ethyl 2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-1-acetate hydrochloride are dissolved in 1 liter of hot water. The pH should be 4-5. When the temperature of the reaction medium is 50° C., a solution of 8.7 g (0.13 mol) of sodium cyanate in 150 cm3 of water is added. The reaction medium is kept at 50° C., whilst stirring. It is stirred for 4 hours at 50° C. and left to stand overnight at ambient temperature; the supernatant water is drawn off. 200 cm3 of ether are added, the mixture is stirred, the ether solution is then drawn off and the same operation is repeated. The expected product is very soluble in ether. The ether extracts are combined and washed with acidified water, in order to remove traces of the starting material, and then with water. They are dried over Na2SO4 and the solvent is evaporated off. This yields an oil which changes into a foam on more thorough drying. The product is used as such in the following step.

Aufarbeitung

  1. customis 50° C.
  2. customis kept at 50° C.
  3. stirringIt is stirred for 4 hours at 50° C.
  4. waitleft
  5. stirringthe mixture is stirred

Quellen und Nachweise

ORD-Eintrag
ord-38cb2051bbe54cafbf743a4aff7f164f
Quelldatensatz
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04358451

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