反应详情

温度

23 °C

To a solution of (R)-4-(3-(3-(bis(4-methoxyphenyl)(phenyl)methylamino)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-5-yl)-4-fluorophenylamino)benzonitrile (intermediate A13A) (21 mg, 31 μmol) in dichloromethane (1 ml) at 23° C. was added trifluoroacetic acid (370 mg, 250 μl, 3.24 mmol) and the mixture was stirred at 23° C. for 1 h. Poured into sat. Na2CO3-sol., extracted thrice with ethyl acetate, dried the combined organic layer over Na2SO4. Removal of the solvent in vacuum left a crude product, which was purified by preparative HPLC (column: Gemini 5μ C18 110 A° AXIA (50×21.2 mm); flow: 40 ml/min; gradient: water (+0.1% TEA)/acetonitrile (90%-10% 1 min plateau; in 3.5 min to 5%-95%); collection: UV-detector 300 nm) to give the title compound (8.9 mg, 76.6%) after trituration with little diethyl ether/pentane as a white solid. MS (ISP): m/z=375.3 [M+H]+.

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5. customwas purified by preparative HPLC (column: Gemini 5μ C18 110 A° AXIA (50×21.2 mm); flow: 40 ml/min; gradient: water (+0.1% TEA)/acetonitrile (90%-10% 1 min plateau; in 3.5 min to 5%-95%); collection: UV-detector 300 nm)