Lithium hydroxide, monohydrate → 3-chloro-1H-pyrrole-2-carboxylic acid
反応式
[Cl:1][C:2]1[CH:6]=[CH:5][NH:4][C:3]=1[C:7]([O:9]C)=[O:8].O[Li].O>CO.O>[Cl:1][C:2]1[CH:6]=[CH:5][NH:4][C:3]=1[C:7]([OH:9])=[O:8]参加物
4
反応条件
- 温度
- 25 °C
実験手順
Methyl 3-chloro-1H-pyrrole-2-carboxylate (18.86 mmol, 1.0 equiv.) was dissolved in MeOH—H2O (2:1, 120 ml); at 0° C., LiOH.H2O (75.4 mmol, 4 equiv.) was added and the mixture was stirred for 16 h at 25° C. The methanol was concentrated under reduced pressure, and the aqueous residue was diluted with water (60 ml) and extracted with ethyl acetate (2×50 ml). The aqueous phase was adjusted to pH 3-4 with 1 M HCl, and the resulting solid was filtered out. Yield: 90%
後処理
- concentrationThe methanol was concentrated under reduced pressure
- additionthe aqueous residue was diluted with water (60 ml)
- extractionextracted with ethyl acetate (2×50 ml)
- filtrationthe resulting solid was filtered out
出典と根拠
- ORDレコード
- ord-6abd48602ed34abcbfbd3df20869cd2b
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08492559B2
反応ノート
読み込み中…