2,3-dihydro-1H-cinnolin-4-one;hydrochloride

Conditions: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 69.41 g of the product obtained in stage A are dissolved in 2.5 l of ethanol. 62.79 g of zinc powder are subsequently added, followed, slowly, by a mixture of 300 ml of ethanol and 150 ml of acetic acid at ambient temperature. The mixture is heated at reflux for 30 min. The reaction medium is subsequently separated by settling, and the zinc residue is washed several times with ethanol. After being allowed to cool for 20 minutes in an ice/methanol mixture (−15° C.), a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M). The precipitate formed is filtered off, washed with ether and then with pentane, and finally dried (under reduced pressure). 42.12 grams (60%) of the expected product are obtained. The mixture is heated at reflux for 30 min The reaction medium is subsequently separated the zinc residue is washed several times with ethanol a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M) The precipitate formed is filtered off washed with ether with pentane, and finally dried (under reduced pressure)

Conditions: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 69.41 g of the product obtained in stage A are dissolved in 2.5 l of ethanol. 62.79 g of zinc powder are subsequently added, followed, slowly, by a mixture of 300 ml of ethanol and 150 ml of acetic acid at ambient temperature. The mixture is heated at reflux for 30 min. The reaction medium is subsequently separated by settling, and the zinc residue is washed several times with ethanol. After being allowed to cool for 20 minutes in an ice/methanol mixture (−15° C.), a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M). The precipitate formed is filtered off, washed with ether and then with pentane, and finally dried (under reduced pressure). 42.12 grams (60%) of the expected product are obtained. The mixture is heated at reflux for 30 min The reaction medium is subsequently separated the zinc residue is washed several times with ethanol a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M) The precipitate formed is filtered off washed with ether with pentane, and finally dried (under reduced pressure)

Conditions: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 69.41 g of the product obtained in stage A are dissolved in 2.5 l of ethanol. 62.79 g of zinc powder are subsequently added, followed, slowly, by a mixture of 300 ml of ethanol and 150 ml of acetic acid at ambient temperature. The mixture is heated at reflux for 30 min. The reaction medium is subsequently separated by settling, and the zinc residue is washed several times with ethanol. After being allowed to cool for 20 minutes in an ice/methanol mixture (−15° C.), a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M). The precipitate formed is filtered off, washed with ether and then with pentane, and finally dried (under reduced pressure). 42.12 grams (60%) of the expected product are obtained. The mixture is heated at reflux for 30 min The reaction medium is subsequently separated the zinc residue is washed several times with ethanol a solution of hydrogen chloride gas in ethyl acetate is then added (350 ml; 4M) The precipitate formed is filtered off washed with ether with pentane, and finally dried (under reduced pressure)