Pyridine → HCID 70548484, Verbindung

HRID 2397276Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2397276
[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 56, 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-8d1e7db6e97e475eb3e159c9cc7d65d3
Quelldatensatz
uspto-grants-1977_05
Patentnummer
US04021451

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