反应 #1810846

反应方程式

2-Amino-4-(1-cyclopropylmethyl-2-methylimidazol-5-yl)pyrimidine

N-(2-methoxyethyl)-N-(t-butyl)-4-iodobenzenesulphonamide

acetic acid

→

title compound

收率 32.2%

4-(1-Cyclopropylmethyl-2-methylimidazol-5-yl)-2-{4-[N-(2-methoxyethyl)-N-(t-butyl)sulphamoyl]anilino}pyrimidine

收率 32.2%

溶剂

water

反应条件

后处理

1. 1
   萃取extracted with EtOAc
2. 2
   洗涤washed with water
3. 3
   干燥brine, dried
4. 4
   其他the solvent removed by evaporation
5. 5
   其他The residue was purified by chromatography on silica gel eluting with DCM/MeOH (97:3)

实验过程

2-Amino-4-(1-cyclopropylmethyl-2-methylimidazol-5-yl)pyrimidine (Method 54; 2 g, 8.73 mmol) was treated with N-(2-methoxyethyl)-N-(t-butyl)-4-iodobenzenesulphonamide (Method 77; 3.82 g, 9.61 mmol) under the conditions described in Example 22. The reaction was quenched by the addition of acetic acid (250 μl, 4.37 mmol), the mixture was poured into water and extracted with EtOAc. The extracts were combined, washed with water and then brine, dried and the solvent removed by evaporation. The residue was purified by chromatography on silica gel eluting with DCM/MeOH (97:3) to give the title compound (1.4 g, 32%) as a pale yellow foam. NMR: 0.01 (m, 2H) 0.18 (m, 2H) 1.90 (m, H) 2.26 (s, 3H) 3.15 (s, 3H) 3.37 (m, 4H) 4.42 (d, 2H) 7.08 (d, H) 7.52 (s, H) 7.58 (d, 2H) 7.75 (d, 2H) 8.30 (d, H) 9.75 (s, H); m/z 499.

来源