Hydrochloric Acid → (5-Bromo-6-methoxy-pyridin-3-yl)-acetic acid
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][C:11]#N)[CH:5]=[N:6][C:7]=1[O:8][CH3:9].[OH-:13].[K+].Cl.[OH2:16]>CCO>[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][C:11]([OH:16])=[O:13])[CH:5]=[N:6][C:7]=1[O:8][CH3:9]参加物
6
反応条件
- 温度
- 80 °C
実験手順
To a suspension of (5-bromo-6-methoxy-pyridin-3-yl)-acetonitrile (Step AM1) (6.61 mmol) in EtOH (19 mL) was added a solution of KOH (26.7 mmol) in H2O (19 mL) and the mixture was stirred at 80° C. for 45 min. After cooling to rt, the pH was adjusted to 3-4 with 1M aqueous HCl and the mixture was extracted with CH2Cl2 (2×). The combined organic layers were dried (MgSO4), filtered and concentrated to afford the title compound. ESI-MS: tR=0.75 min, [M+H]+ 246/248 (LC-MS 1).
後処理
- temperatureAfter cooling to rt
- extractionthe mixture was extracted with CH2Cl2 (2×)
- dry with materialThe combined organic layers were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-853c5cd6c14c4984be132999887ea759
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365576B2
反応ノート
読み込み中…