Lithium Hydroxide → HCID 67691019, 화합물

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To a solution of trans-2-methoxycarbonyl-5,7-dichloro-4-(3-tert-butyloxycarbonylaminomethylphenyl)carbonylamino-1,2,3,4-tetrahydroquinoline (step b) (430 mg, 0.846 mmol) in a mixture of tetrahydrofuran (20 ml) and water (10 ml) was added aqueous lithium hydroxide (1.95 ml of a 0.5M solution, 0.973 mmol), and the resulting mixture was stirred at room temperature for 3 h. The organic solvent was removed in vacuo and the aqueous residue was diluted to 50 ml before acidifying to pH 1 with 1N HCl. The white precipitate was extracted into ethyl acetate (150 ml), washed with brine and dried (Na2SO4). The solution was evaporated to give a residue which was washed with diethyl ether and collected by filtration to give the title compound as a colourless crystalline solid, m.p. 192°-193° C. δ (DMSO, 360 MHz) 1.39 (9H, s, C(CH3)3, 1.73 (1H, ddd, 13.2, 13.0 and 3.8 Hz, CHACHBHCCHD), 2.26 (1H, dm, J=13.2 Hz, CHACHBHCCHD), 3.96 (1H, dd, J=13.0 and 3.0 Hz, CHACHBHCCHD), 4.14 (2H, d,J=5.6 Hz, ArCH2NH), 5.26 (1H, m, CHACHBHCCHD), 6.65 (1H, d, J=2.0 Hz, 6-H or 8-H), 6.82 (1H, br s, ArNHCO), 6.91 (1H, d, J=2.0 Hz, 6-H or 8-H). 7.36-7.37 and 7.72-7.76 (5H, m, Ar-H and CH2NHCO), 8.66 (1H, d, J=7 Hz, NHCOAr); m/e (FAB+), 494 (M+1), 93 (100%); Found C, 55.92; H, 5.22; N, 8.35; C23H25Cl2N3O5 requires C, 55.88; H, 5.10; N, 8.50%.

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