Reaktion #1269159

Reaktionsgleichung

4-[4-({1-[8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromen-2-yl]-methanoyl}-amino)-phenyl]-piperazine-1-carboxylic acid tert-butyl ester

→

solid

Ausbeute 76.0%

8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid (4-piperazin-1-yl-phenyl)-amide

Ausbeute 76.0%

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeHCl gas was bubbled in slowly for 2 minutes
2. 2
   Sonstigeto precipitate
3. 3
   workup.ADDITIONMethanol (3-4 mL) was added
4. 4
   workup.DISSOLUTIONto dissolve this solid and HCl gas
5. 5
   Sonstigewas bubbled in for another 2 minutes
6. 6
   EinengenThe mixture was concentrated under reduced pressure
7. 7
   Sonstigetriturated with ether
8. 8
   Sonstigedried under vacuum

Vorschrift

4-[4-({1-[8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromen-2-yl]-methanoyl}-amino)-phenyl]-piperazine-1-carboxylic acid tert-butyl ester (Example 29) (160 mg, 0.3 mmol) was dissolved ethyl acetate (20 mL) and cooled to 0° C. HCl gas was bubbled in slowly for 2 minutes. A solid began to precipitate. Methanol (3-4 mL) was added to dissolve this solid and HCl gas was bubbled in for another 2 minutes. The mixture was concentrated under reduced pressure and triturated with ether and dried under vacuum to yield a tan solid (100 mg, 76%). LCMS/m/z=448.6.

Quelle