Lithium Hydroxide → HCID 86707798、化合物
反応式
C[O:2][C:3]([CH:5]1[CH2:8][N:7]([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH2:19][C:18]([C:24]4[CH:29]=[C:28]([Cl:30])[C:27]([Cl:31])=[C:26]([Cl:32])[CH:25]=4)([C:20]([F:23])([F:22])[F:21])[O:17][N:16]=3)=[CH:11][C:10]=2[Cl:33])[CH2:6]1)=[O:4].[OH-].[Li+]>C1COCC1.CO.O>[Cl:33][C:10]1[CH:11]=[C:12]([C:15]2[CH2:19][C:18]([C:24]3[CH:25]=[C:26]([Cl:32])[C:27]([Cl:31])=[C:28]([Cl:30])[CH:29]=3)([C:20]([F:22])([F:23])[F:21])[O:17][N:16]=2)[CH:13]=[CH:14][C:9]=1[N:7]1[CH2:6][CH:5]([C:3]([OH:4])=[O:2])[CH2:8]1参加物
4
実験手順
To a stirred suspension of 1-{2-Chloro-4-[5-(3,4,5-trichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-phenyl}-azetidine-3-carboxylic acid methyl ester (Preparation 13, 0.55 g, 1.086 mmol) in THF:MeOH:H2O (1:1:1, 9 mL) was added lithium hydroxide (0.228 g, 5.43 mmol) at room temperature. Resulting reaction mixture was stirred at room temperature for 18 hours. After consumption of starting material, reaction mixture was concentrated in vacuo; acidified with 1N HCl up to pH ˜5. Acidified aqueous layer was extracted with ethyl acetate (5×20 mL). Combined organic layer was dried over sodium sulphate and evaporated under reduced pressure and was triturated with n-pentane (25 mL) to afford off white solid (0.4 g, 74%). 1H NMR (400 MHz, DMSO-d6) δ: 3.45-3.50 (m, 1H), 4.12-4.16 (m, 2H), 4.26-4.33 (m, 4H), 6.67 (d, 1H, J=9.04 Hz), 7.51-7.53 (m, 2H), 7.81 (s, 2H), 12.75 (bs, 1H); LC-MS (M+H): =528.80.