Ammonium Chloride → HCID 135737584, compound

Participants

Reaction Steps

5.0 g (0.022 mole) of the methyl ketone 2acetylpyrazolo[1,5-c]quinazolin-5(6H)-one prepared as in Example 4A is suspended under argon in dry distilled tetrahydrofuran (100 ml) and treated quickly with 7.0 ml (~1.0 equivalent) of 3M C6H5MgBr/ethyl ether. The mixture is stirred for 5 minutes and another 15 ml (~2 equivalents) of the Grignard reagent is quickly added. The reaction mixture (dark brown) is stirred at room temperature for 30 minutes and then refluxed for another 30 minutes, cooled down to room temperature and the resulting reddish solution is treated with 8.0 ml of saturated NH4Cl solution. The mixture is diluted with 70 ml tetrahydrofuran and stirred at room temperature for ~1 hour. The inorganic salts are filtered off and washed well with tetrahydrofuran (30 ml) and CHCl3 (50 ml). The filtrates are combined and stripped to dryness. Yield: 8.4 g; 3 spots on TLC.

Provenance & Evidence