Pyridine → HCID 70548484, Verbindung

HRID 1703350Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1703350
[CH3:1][O:2][CH:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH:8]3[CH2:13][CH2:14][O:15][C:6]([C:7]=23)=[CH:5][N:4]1[O:16][CH3:17].[C:18](OC(=O)C)(=[O:20])[CH3:19].N1C=CC=CC=1>O>[C:18]([CH:10]1[CH2:11][C:12]2[CH:3]([O:2][CH3:1])[N:4]([O:16][CH3:17])[CH:5]=[C:6]3[O:15][CH2:14][CH2:13][CH:8]([C:7]=23)[CH2:9]1)(=[O:20])[CH3:19]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 20523931HCID 20523931, Verbindung

Produkt 1

HCID 70548484HCID 70548484, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 1,2,3a,4,5,6-hexahydro-7,8-dimethoxypyrano-[2,3,4-de]isoquinoline (10.0 g), described in Example 23, acetic anhydride (60.0 ml) and pyridine (0.5 ml) is heated on the steam bath for 4 hr. The mixture is poured into water and stirred for 2 hr. The mixture is extracted with chloroform and the extracts are washed with sodium bicarbonate solution and then with brine. The organic solution is dried and evaporated to leave the title compound. A sample, crystallized from isopropanol, had m.p. 100°-102° C.

Aufarbeitung

  1. temperatureis heated on the steam bath for 4 hr
  2. extractionThe mixture is extracted with chloroform
  3. washthe extracts are washed with sodium bicarbonate solution
  4. customThe organic solution is dried
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-afac6593aca54cfc886fbf22f79608d7
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04351942

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