Lithium hydroxide, monohydrate → 4-(6-Chloropyridin-3-yl)benzoic acid
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:17]=[CH:16][C:11]([C:12]([O:14]C)=[O:13])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.O[Li].O>C1COCC1.O>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:17]=[CH:16][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1参加物
5
実験手順
A solution of Example 252F (1.56 g, 6.4 mmol) in THF (30 mL) at room temperature was treated with a solution of LiOH.H2O (0.537 g, 12.8 mmol) in water (5 mL), heated to reflux for 4 hours, cooled to room temperature and concentrated. The mixture was neutralized with 1N HCl and extracted ethyl acetate (3×50 nL). The combined extracts were washed with brine, dried (Na2SO4), filtered, and concentrated to provide the desired product. MS (APCI) m/e 234 (M+H)+.
後処理
- temperatureheated
- temperatureto reflux for 4 hours
- concentrationconcentrated
- extractionextracted ethyl acetate (3×50 nL)
- washThe combined extracts were washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-eb61d8f2c13945b489d671415d180861
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07504512B2
反応ノート
読み込み中…