Hydrochloric Acid → N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamide

HRID 1648281Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1648281
[OH-].[Na+].[O:3]=[C:4]1[C:13]([NH:19][CH:20]=[O:21])(C(OCC)=O)[CH2:12][C:11]2=[CH:22][CH:23]=[CH:24][C:9]3=[C:10]2[N:5]1[CH2:6][CH2:7][CH2:8]3.Cl>CO>[O:3]=[C:4]1[CH:13]([NH:19][CH:20]=[O:21])[CH2:12][C:11]2=[CH:22][CH:23]=[CH:24][C:9]3=[C:10]2[N:5]1[CH2:6][CH2:7][CH2:8]3

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86747427ethyl 2,3,6,7-tetrahydro-3-oxo-2-(formylamino)-1H,5H-benzo(ij)quinolizine-2-carboxylate

Produkt 1

HCID 19919292N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamideAusbeute 104,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Sodium hydroxide solution (5.0 mL of 4.0 N, 20 mmol) was slowly added to ethyl 2,3,6,7 - tetrahydro- 3 -oxo -2- (formyl amino) - 1H,5 H-benzo(ij )quinolizine-2-carboxyl ate (3.134 g, 10.0 mmol) in methanol (25 mL). After stirring at room temperature for 30 rain, hydrochloric acid (5.0 mL of 4.0 N) was added and the precipitate was filtered off, washed with water and air dried to give 2.4 g of N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamide, mp 149°-152° C. A portion of the product was recrystallized from ethyl acetate for analysis; mp 140-143° . Anal. Calc'd for C13H14N2O2 : C, 67.81; H, 6.13; N, 12.17. Found: C, 67.67; H, 6.07; N, 11.94.

Aufarbeitung

  1. additionwas added
  2. filtrationthe precipitate was filtered off
  3. washwashed with water and air
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-732c333f4c1b424c99d169beb948e29f
Quelldatensatz
uspto-grants-1995_07
Patentnummer
US05436240

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