Sodium Hydroxide → Sodium 3-(5-{5-[3-chloro-4-(ethyloxy)phenyl]-1,2,4-oxadiazol-3-yl}-1H-indazol-1-yl)propanoate
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2[O:15][N:14]=[C:13]([C:16]3[CH:17]=[C:18]4[C:22](=[CH:23][CH:24]=3)[N:21]([CH2:25][CH2:26][C:27]([O:29]CC)=[O:28])[N:20]=[CH:19]4)[N:12]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH3:10].[OH-].[Na+:33]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2[O:15][N:14]=[C:13]([C:16]3[CH:17]=[C:18]4[C:22](=[CH:23][CH:24]=3)[N:21]([CH2:25][CH2:26][C:27]([O-:29])=[O:28])[N:20]=[CH:19]4)[N:12]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH3:10].[Na+:33]参加物
4
反応条件
- 温度
- 50 °C
実験手順
Ethyl 3-(5-{5-[3-chloro-4-(ethyloxy)phenyl]-1,2,4-oxadiazol-3-yl}-1H-indazol-1-yl)propanoate (D57) (77 mg, 0.17 mmol) was suspended in 2M aq. NaOH (2 ml) and ethanol (2 ml). The mixture was heated at 50° C. until dissolved then cooled. The ethanol was removed in vacuo and the resultant solid was filtered, washed with ethanol, water and diethyl ether then dried under high vacuum to afford the title compound (63.6 mg) as a pink solid. δH (methanol-d4, 400 MHz) 1.49 (3H, t), 2.77 (2H, t), 4.25 (2H, q), 4.71 (2H, t), 7.27 (1H, d), 7.82 (1H, d), 8.09-8.25 (4H, m), 8.55 (1H, s). MS (ES): C20H1735ClN4O4 requires; 412 found (MH+) 413.
後処理
- dissolutionuntil dissolved
- temperaturethen cooled
- customThe ethanol was removed in vacuo
- filtrationthe resultant solid was filtered
- washwashed with ethanol, water and diethyl ether
- customthen dried under high vacuum
出典と根拠
- ORDレコード
- ord-52c92034f03f4134a1d2d6053d5421db
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08324254B2
反応ノート
読み込み中…