2-amino-5-bromo-3-methoxybenzaldehyde

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 2-amino-5-bromo-3-methoxybenzaldehyde (2.5 g, 10.87 mmol) is homogeneously mixed with urea and the mixture is heated to 180° C. The melt formed is kept at this temperature for 1 h. Then the reaction mixture is mixed with water, the precipitate formed is filtered off, dried and 6-bromo-8-methoxy-1H-quinazolin-2-one (HPLC-MS: tRet.=1.53 min MS(M+H)+=255/257; method FSUN) is obtained. The melt formed the precipitate formed is filtered off dried

Conditions: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The mixture of 2-amino-5-bromo-3-methoxybenzaldehyde (43.96 mmol, crude material from step 3) and urea (35 g, 583 mmol) from the previous step was heated to 180° C. under argon for 1 hour. Water (300 mL) was added after cooling to room temperature. The solid was collected by filtration and air dried to give 12.45 g of powder. ES/MS m/z 254/256 (MH+). after cooling to room temperature The solid was collected by filtration and air dried

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

Procedure: To a 0.15 M chloroform solution of (2-amino-5-bromo-3-methoxyphenyl)methanol (10.16 g, 43.96 mmol) was added manganese dioxide (19.9 g, 280.5 mmol). The mixture was stirred under argon at room temperature for 16 hours. The resulting mixture was filtered through celite and washed with dichloromethane. The filtrate was concentrated to dryness and used in next step. ES/MS m/z 228/230 (MH+). The resulting mixture was filtered through celite washed with dichloromethane The filtrate was concentrated to dryness

Conditions: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 2-amino-5-bromo-3-methoxybenzaldehyde (2.5 g, 10.87 mmol) is homogeneously mixed with urea and the mixture is heated to 180° C. The melt formed is kept at this temperature for 1 h. Then the reaction mixture is mixed with water, the precipitate formed is filtered off, dried and 6-bromo-8-methoxy-1H-quinazolin-2-one (HPLC-MS: tRet.=1.53 min MS(M+H)+=255/257; method FSUN) is obtained. The melt formed the precipitate formed is filtered off dried