Reaktion #1903412

Reaktionsgleichung

sodium hydride

4-amino-3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinoline

ammonium chloride

methyl 2-oxo-1-pyrrolidine acetate

→

titled compound

Ausbeute 83.5%

2-(2-oxopyrrolidin-1-yl)-N-(3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinolin-4-yl)acetamide

Ausbeute 83.5%

Lösungsmittel

N-ethylpyrrolidone

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated to 50.degree
2. 2
   workup.WAITover a period of 30 minutes
3. 3
   workup.WAITfor 20 minutes
4. 4
   Temperaturthe mixture was cooled to 15.degree
5. 5
   ExtraktionAfter extraction of the solution with 100 ml of chloroform
6. 6
   Trocknenthe extract was dried over anhydrous sodium sulfate
7. 7
   Sonstigefollowed by evaporation to dryness
8. 8
   workup.ADDITIONThe resultant product was added with ethyl acetate
9. 9
   Filtrationfiltered
10. 10
    SonstigeThe crude crystals were recrystallized from chloroform-ethyl acetate

Vorschrift

Into a suspension of 1.26 g of sodium hydride (60% content) in 15 ml of N-ethylpyrrolidone, was added 3.28 g of 4-amino-3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinoline at room temperature. The mixture was heated to 50.degree. C. and stirred for 40 minutes. Thereafter, 4.72 g of methyl 2-oxo-1-pyrrolidine acetate was added dropwise to the mixture at 50.degree. C. over a period of 30 minutes. After the stirring at 50.degree. C. for 20 minutes, the mixture was cooled to 15.degree. C. and poured into 130 ml aqueous solution containing 13.5 g of ammonium chloride. After extraction of the solution with 100 ml of chloroform, the extract was dried over anhydrous sodium sulfate, followed by evaporation to dryness. The resultant product was added with ethyl acetate, pulverized and filtered. The crude crystals were recrystallized from chloroform-ethyl acetate to obtain 4.31 g of the titled compound having the melting point of 244.degree. to 246.degree. C.

Quelle