反应详情

A solution of the product of Example 1 (200 mg) in methanol (10 ml), prepared under argon, was cooled to 4° C. and saturated with dry ammonia gas, then sealed in a pressure bottle and kept for 2 days. The orange crystals which formed, after filtration and washing with a little methanol, gave the title compound, 140 mg: m.p. 247° to 248° C.; NMR (d6DMSO)δ8.16(2H,d), 7.99(2H,d), 7.55(1H,bs), 7.37(1H,bs), 7.02(2H,d), 6.81(2H,d), 4.54(2H,s), 3.85(2H,s), 3.33(4H,t), 2.60(4H,t); m/e 355 (M+H)+ ; calculated for C19H22N4O3 : C, 64.4; H, 6.3; N, 15.8. found: C, 64.4; H, 6.4; N, 15.6%.

1. customsealed in a pressure bottle
2. customThe orange crystals which formed
3. filtrationafter filtration
4. washwashing with a little methanol