Lithium Hydroxide → HCID 178524007、化合物
反応式
[OH-].[Li+].[F:3][C:4]1[C:5]([NH:20][CH:21]2[CH:27]3[CH2:28][CH2:29][CH:23]([CH2:24][CH2:25][CH2:26]3)[CH:22]2[C:30]([O:32]C)=[O:31])=[N:6][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[C:16]([F:19])[CH:17]=3)[NH:12][N:11]=2)=[N:8][CH:9]=1>C1COCC1>[F:3][C:4]1[C:5]([NH:20][CH:21]2[CH:27]3[CH2:28][CH2:29][CH:23]([CH2:24][CH2:25][CH2:26]3)[CH:22]2[C:30]([OH:32])=[O:31])=[N:6][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[C:16]([F:19])[CH:17]=3)[NH:12][N:11]=2)=[N:8][CH:9]=1参加物
4
反応条件
- 温度
- 85 °C
実験手順
A solution of lithium hydroxide (2.10 mL of 2N solution, 4.15 mmol) was added to a stirred solution of racemic methyl 7-(5-fluoro-2-(5-fluoro-1H-pyrazolo[3,4-b]pyridin-3-yl)pyrimidin-4-ylamino)bicyclo[3.2.2]nonane-6-carboxylate, I-36, (0.18 g, 0.42 mmol) in THF (7 mL). The solution was heated at 85° C. for 6 hr and cooled to room temperature. The solution was concentrated in vacuo and water (5 mL) was added. The solution was slowly neutralized with 1N HCl to produce a white precipitate. The precipitate was filtered and washed with water (10 mL). The wet solid was lyophilized for 2 days to 112 mg of the desired product as a white powder: 1H NMR (400 MHz, CD3OD) δ 8.77 (s, 1H), 8.52 (s, 1H), 8.10 (s, 1H), 5.29 (m, 1H), 2.82 (m, 1H), 2.53 (m, 1H), 2.11-1.54 (brm, 10H), 1.29 (m, 1H); LC/MS Gradient 10-90%, 0.1% formic 5 min, C18/ACN, RT=2.33 minutes (M+H) 415.44.