反応 #1973977

反応方程式

product

1-(3-(2-aminobenzo[d]thiazol-6-yl)-5-tert-butyl-4-methoxy-phenyl)pyrimidine-2,4(1H,3H)-dione

methanesulfonyl chloride

pyridine

→

title compound

収率 4.6%

N-(6-(3-tert-butyl-5-(2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)-2-methoxyphenyl)benzo[d]thiazol-2-yl)methanesulfonamide

収率 4.6%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   その他The crude product was purified by C-18 reverse-phase

実験手順

To a solution of the product from Example 53 (0.35 g, 0.83 mmol) in anhydrous CH2Cl2 (50 mL) was added methanesulfonyl chloride (194 μL, 2.49 mmol) and pyridine (1.34 mL, 16.6 mmol). The resulting mixture was stirred at room temperature for 16 h and concentrated in vacuo. The crude product was purified by C-18 reverse-phase HPLC using an acetonitrile:H2O (0.1% TFA) gradient to give the title compound (19 mg, 4%). 1H NMR (300 MHz, DMSO-d6) δ 13.09 (s, 1 H) 11.41 (d, J=1.84 Hz, 1 H) 7.96 (d, J=1.47 Hz, 1 H) 7.77 (d, J=8.09 Hz, 1 H) 7.57 (dd, 1 H) 7.42 (d, J=8.09 Hz, 1 H) 7.25-7.32 (m, 2 H) 5.64 (dd, J=8.09, 2.21 Hz, 1 H) 3.25 (s, 3 H) 3.02 (s, 3 H) 1.40 (s, 9 H).

出典