反应详情

N-[(3S)-1-[6-Chloro-5-[[(cyclohexylmethyl)amino]carbonyl]-2-quinolinyl]-3-pyrrolidinyl]-N-[[[(1,1-dimethylethoxy)carbonyl]amino]sulfonyl]-glycine, ethyl ester (Example 112 (b)) (670 mg) was dissolved in dichloromethane (5 mL). Trifluoroacetic acid (1 mL) was added and the mixture stirred for 3 hours before being concentrated. Sodium methoxide (25% in methanol, 3 mL) was added and the mixture was stirred under nitrogen for 2 hours. The products were concentrated onto silica gel and purified by chromatography (SiO2, dichloromethane:methanol 92:8 as eluant). Further purification by HPLC (Symmetry—0.1% aqueous trifluoroacetic acid/acetonitrile) gave the title compound as a solid (20 mg).

1. concentrationbefore being concentrated
2. additionSodium methoxide (25% in methanol, 3 mL) was added
3. stirringthe mixture was stirred under nitrogen for 2 hours
4. concentrationThe products were concentrated onto silica gel
5. custompurified by chromatography (SiO2, dichloromethane:methanol 92:8 as eluant)
6. customFurther purification by HPLC (Symmetry—0.1% aqueous trifluoroacetic acid/acetonitrile)