反应详情

Using similar reaction conditions as described in step-iii of example-1, N-(5-(3-(1-(3-fluorobenzyl)-1H-pyrazol-4-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-5-yl)-2-methoxypyridin-3-yl) methanesulfonamide (70 mg, 0.108 mmol) was hydrolyzed with lithium hydroxide (14 mg, 0.324 mmol) in THF/methanol/water (3.5/3.5/0.5 mL) to yield 17 mg (31.8% yield) after purification by preparative TLC (Silicagel-1000 micron) using 5% methanol in chloroform as eluent. 1H NMR (CD3OD, 300 MHz): δ 8.42 (s, 1H), 8.34-8.33 (s, 1H), 8.288-8.280 (d, 1H), 8.22 (s, 1H), 8.04-8.03 (d, 1H), 7.934-7.931 (d, 1H), 8.04-8.03 (d, 1H), 7.934-7.931 (d, 1H), 7.65 (s, 1H), 7.38-7.35 (q, 1H), 7.12-7.09 (d, 1H), 7.03-6.99 (m, 2H), 5.42 (s, 2H), 4.06 (s, 3H), 3.03 (s, 3H). MS: m/z=492.8 (M+1), HPLC: 96.33% in method B.

1. customreaction conditions
2. customto yield 17 mg (31.8% yield)
3. customafter purification by preparative TLC (Silicagel-1000 micron)