8-bromo-3,4-dihydro-1H-quinoxalin-2-one

Conditions: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A sealable tube is charged with 4.99 g (39.549 mmol) of a mixture of 8-Bromo-3,4-dihydro-1H-quinoxalin-2-one with (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester (as obtained in step 1.2). 50 mL of a 1M NaOH solution and 12.1 ml of a 30% H2O2 aqueous solution are added. The tube is sealed and heated to 95° C. for 1 h. After cooling, 50 mL of 1M HCl solution are added slowly and the brown solid is collected by filtration, to afford, after drying in HV at 50° C., the title compound which is used without further purification. The tube is sealed After cooling the brown solid is collected by filtration to afford after drying in HV at 50° C. the title compound which is used without further purification

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

Procedure: 10.33 g (ca. 25.9 mmol) (3-Bromo-2-nitro-phenylamino)-acetic acid ethyl ester is hydrogenated in the presence of 2.84 g Ra—Ni (B113W EtOH, Degussa) in 340 ml of THF:EtOH=1:1 for 20 h. The reaction mixture is filtered on hyflo and the filtrate is concentrated in vacuo. A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained and used as obtained in the next synthetic step. The reaction mixture is filtered on hyflo the filtrate is concentrated in vacuo A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained as obtained in the next synthetic step

Conditions: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A sealable tube is charged with 4.99 g (39.549 mmol) of a mixture of 8-Bromo-3,4-dihydro-1H-quinoxalin-2-one with (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester (as obtained in step 1.2). 50 mL of a 1M NaOH solution and 12.1 ml of a 30% H2O2 aqueous solution are added. The tube is sealed and heated to 95° C. for 1 h. After cooling, 50 mL of 1M HCl solution are added slowly and the brown solid is collected by filtration, to afford, after drying in HV at 50° C., the title compound which is used without further purification. The tube is sealed After cooling the brown solid is collected by filtration to afford after drying in HV at 50° C. the title compound which is used without further purification

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

Procedure: 10.33 g (ca. 25.9 mmol) (3-Bromo-2-nitro-phenylamino)-acetic acid ethyl ester is hydrogenated in the presence of 2.84 g Ra—Ni (B113W EtOH, Degussa) in 340 ml of THF:EtOH=1:1 for 20 h. The reaction mixture is filtered on hyflo and the filtrate is concentrated in vacuo. A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained and used as obtained in the next synthetic step. The reaction mixture is filtered on hyflo the filtrate is concentrated in vacuo A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained as obtained in the next synthetic step

Conditions: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A sealable tube is charged with 4.99 g (39.549 mmol) of a mixture of 8-Bromo-3,4-dihydro-1H-quinoxalin-2-one with (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester (as obtained in step 1.2). 50 mL of a 1M NaOH solution and 12.1 ml of a 30% H2O2 aqueous solution are added. The tube is sealed and heated to 95° C. for 1 h. After cooling, 50 mL of 1M HCl solution are added slowly and the brown solid is collected by filtration, to afford, after drying in HV at 50° C., the title compound which is used without further purification. The tube is sealed After cooling the brown solid is collected by filtration to afford after drying in HV at 50° C. the title compound which is used without further purification

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

Procedure: 10.33 g (ca. 25.9 mmol) (3-Bromo-2-nitro-phenylamino)-acetic acid ethyl ester is hydrogenated in the presence of 2.84 g Ra—Ni (B113W EtOH, Degussa) in 340 ml of THF:EtOH=1:1 for 20 h. The reaction mixture is filtered on hyflo and the filtrate is concentrated in vacuo. A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained and used as obtained in the next synthetic step. The reaction mixture is filtered on hyflo the filtrate is concentrated in vacuo A mixture of the title compound with uncyclized (2-Amino-3-bromo-phenylamino)-acetic acid ethyl ester is obtained as obtained in the next synthetic step