反应详情

A solution of 2-(3-{6-[2-(2,4-dichloro-phenyl)-ethylamino]-2-methoxy-pyrimidin-4-yl}-phenyl)-2-methyl-propionic acid [4.3 g, 9.35 mmol, Example 49(b)] in MeOH is treated with 1 M hydrogen chloride in ether (18 mL). The mixture is evaporated and the resulting oil is dissolved in acetone (10 mL). After 2 minutes a solid precipitated. This is filtered giving 2-(3-{6-[2-(2,4-Dichloro-phenyl)-ethylamino]-2-methoxy-pyrimidin-4-yl}-phenyl)-2-methyl-propionic acid hydrochloride [4.043 g, 87%, Example 15(d)] as a solid. LC/MS: RT=2.42 minutes, MS: 460 (M+H). 1H NMR [(CD3)2SO]: □ 12.4 (1H, br s), 7.36-7.8 (7H, m), 6.6 (1H, s), 4 (3H, s), 3.7 (2H, m), 3.02 (2H, m), 1.54 (6H, s). IC50=0.3 nM

1. customThe mixture is evaporated
2. dissolutionthe resulting oil is dissolved in acetone (10 mL)
3. customAfter 2 minutes a solid precipitated
4. filtrationThis is filtered