Water → HCID 67229016, 화합물

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C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:20]([O:27][C:28](=[O:43])[NH:29][C:30]1[C:39]2[CH2:38][CH:37]([N:40]=[N+]=[N-])[CH2:36][CH2:35][C:34]=2[CH:33]=[CH:32][CH:31]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O>C1COCC1>[CH2:20]([O:27][C:28](=[O:43])[NH:29][C:30]1[C:39]2[CH2:38][CH:37]([NH2:40])[CH2:36][CH2:35][C:34]=2[CH:33]=[CH:32][CH:31]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

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실험 절차

Polymer supported triphenylphosphine (9.5 g, 28 mmol) was added to the product of Example 20B (4.6 g, 14 mmol) in THF (100 mL) containing 1.3 g (71 mmol) H2O. The mixture was stirred for 48 hours at ambient temperature, then diluted with THF and filtered through a pad of celite. The filter cake was washed with 3 solvents systems sequentially comprising 100% CH3OH, 1:1 CH3OH:CH2Cl2, and 100% CH2Cl2. The filtrate was concentrated under reduced pressure to provide 3.5 g (83%) of the title compound. 1H NMR (DMSO-d6) δ 8.81 (s, 1H), 7.45-7.30 (m, 5H), 7.13 (d, J=8 Hz, 1H), 7.05 (t, J=7 Hz, 1H), 6.90 (d, J=7 Hz, 1H), 5.12 (s, 2H), 3.00-2.65 (m, 4H), 2.23 (m, 1H), 1.84 (m, 1H), 1.59 (br s, 2H), 1.37 (m, 1H); MS (ESI+) m/z 297 (M+H)+.