Pyridine → HCID 70548484, Verbindung

HRID 259115Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 259115
[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-e80aabcd89e34ccab2368d8b37109df6
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04036842

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