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With dmap In tetrahydrofuran; water at 20℃; for 3 h;
Intermediate 6AH: 4- fcr<-Butoxycarbonylamino)pyridine-3-carboxylic acidTo a stirred solution of 4-aminopyridine-3-carboxylic acid (1.0 g, 7.2 mmol), Boc anhydride in THF: water (1: 1, 20mL) was added DMAP and stirred for 3 h at room temperature. To this was added ethyl acetate (25 mL) and water (25 mL). Aqueous layer was separated, extracted with ethyl acetate (25 mL). Combined organic layer was washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish 1.2 g (69percent) of 4-(ieri-butoxycarbonylamino)pyridine-3-carboxylic acid.MS (ES) m/z 239.1 (M+l).
69%
With dmap In tetrahydrofuran; water at 20℃; for 3 h;
To a stirred solution of 4-aminopyridine-3-carboxylic acid (1.0 g, 7.2 mmol), Boc anhydride in THF:water (1:1, 20 mL) was added DMAP and stirred for 3 h at room temperature. To this was added ethyl acetate (25 mL) and water (25 mL). Aqueous layer was separated, extracted with ethyl acetate (25 mL). Combined organic layer was washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish 1.2 g (69percent) of 4-(tert-butoxycarbonylamino)pyridine-3-carboxylic acid. [0349] MS (ES) m/z 239.1 (M+1)
4-Amino nicotinic acid. A mixture of 4-(N-t-butoxycarbonylamino) nicotinic acid (2.72 g, 11.4 mmol), TFA (10 mL), and CH2 Cl2 (20 mL) is stirred at room temperature for 12 h. The volatiles are removed under reduced pressure, and the resulting crude 4-amino nicotinic acid is used directly in the next reaction. 3H-Pyrido[4,3-d]pyrimidin-4-one.
With dmap; In tetrahydrofuran; water; at 20℃; for 3h;
Intermediate 6AH: 4- fcr<-Butoxycarbonylamino)pyridine-3-carboxylic acidTo a stirred solution of 4-aminopyridine-3-carboxylic acid (1.0 g, 7.2 mmol), Boc anhydride in THF: water (1: 1, 20mL) was added DMAP and stirred for 3 h at room temperature. To this was added ethyl acetate (25 mL) and water (25 mL). Aqueous layer was separated, extracted with ethyl acetate (25 mL). Combined organic layer was washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish 1.2 g (69%) of 4-(ieri-butoxycarbonylamino)pyridine-3-carboxylic acid.MS (ES) m/z 239.1 (M+l).
69%
With dmap; In tetrahydrofuran; water; at 20℃; for 3h;
To a stirred solution of 4-aminopyridine-3-carboxylic acid (1.0 g, 7.2 mmol), Boc anhydride in THF:water (1:1, 20 mL) was added DMAP and stirred for 3 h at room temperature. To this was added ethyl acetate (25 mL) and water (25 mL). Aqueous layer was separated, extracted with ethyl acetate (25 mL). Combined organic layer was washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish 1.2 g (69%) of 4-(tert-butoxycarbonylamino)pyridine-3-carboxylic acid. [0349] MS (ES) m/z 239.1 (M+1)
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