Diethyl Carbonate → HCID 908572, Verbindung

HRID 745301Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 745301
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9](=[CH:15][C:16](=[O:18])[NH2:17])[NH:8][CH2:7][CH2:6]2.[O-:19][CH2:20]C.[Na+].C(=O)(OCC)OCC>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16](=[O:18])[NH:17][C:20](=[O:19])[N:8]1[CH2:7][CH2:6]2

Komponenten

5

Edukt 3

HCID 7766Diethyl CarbonateHCID 2723922Sodium ethoxideHCID 704697252-(6,7-Dimethoxy-3,4-dihydroisoquinolin-1(2H)-ylidene)acetamide

Produkt 1

HCID 908572HCID 908572, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 6,7-dimethoxy-1-carbamoylmethylene-1,2,3,4-tetrahydroisoquinoline (5.0 g) and an excess of sodium ethoxide (prepared from 12.0 g of sodium metal and 600 ml of ethanol) in ethanol is heated. 150.0 ml of diethyl carbonate is added to the solution. The reaction mixture is refluxed for an additional 2.5 hr. The solvent is removed under vacuum and the residue is acidified to give a white precipitate, yield 4.80 g. The product crystallizes from dimethylformamide, mp. 323°-325° C.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for an additional 2.5 hr
  2. customThe solvent is removed under vacuum
  3. customto give a white precipitate, yield 4.80 g
  4. customThe product crystallizes from dimethylformamide, mp. 323°-325° C.

Quellen und Nachweise

ORD-Eintrag
ord-f4de5f0e38ed4bb1a6e1f1894e99435c
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04598148

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