反应详情

(S)-methyl 2-(3-(4-(3-(2-fluorophenyl)ureido)phenyl)-N-methylisoxazole-5-carboxamido)-3-methylbutanoate (80 mg, 0.17 mmol) was dissolved in THF and water in 2:1 ratio. Lithium hydroxide monohydrate (14 mg, 0.341 mmol) was added and the reaction mixture was stirred at room temperature for 6 hours. The reaction mixture was acidified with dilute HCl and extracted with EtOAc. Organic layer was separated, dried over Na2SO4 and concentrated under reduced pressure to yield 30 mg (39%) of the title compound. MS: ES (−): m/z 453 (M−1); ES (+): m/z 455(M+1); 1HNMR (DMSO-d6, 300 MHz) δ: 9.427(s, 1H), 8.713 (d, 1H), 8.171 (m, 1H), 7.905-7.851 (d, 2H), 7.677-7.524 (m, 3H), 7.283 (m, 1H), 7.183 (t, 1H), 7.068 (m, 1H), 4.661-3.949 (d, 1H), 3.161-2.977 (s, 3H), 2.314 (m, 1H), 1.335-1.065 (d, 3H(×2)).

1. extractionextracted with EtOAc
2. customOrganic layer was separated
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure