Lithium Hydroxide → 3-(2-Bromo-thiazol-4-yl)-acrylic acid
反応式
C[O:2][C:3](=[O:12])[CH:4]=[CH:5][C:6]1[N:7]=[C:8]([Br:11])[S:9][CH:10]=1.[OH-].[Li+]>O1CCCC1.O>[Br:11][C:8]1[S:9][CH:10]=[C:6]([CH:5]=[CH:4][C:3]([OH:12])=[O:2])[N:7]=1参加物
5
実験手順
Dissolve 3-(2-bromo-thiazol-4-yl)-acrylic acid methyl ester (5.9 g, 23.78 mmol) in tetrahydrofuran (48 mL) and add a solution of lithium hydroxide (636 mg, 26.16 mmol) in water (10 mL). Stir the mixture overnight. Extract the mixture with ethyl acetate and wash twice with water. Acidify the aqueous layer with 1N HCl in water until the mixture is at pH 3-4. Filter the resulting white solid, then wash the solid with ethyl acetate, followed by diethyl ether and then water. Dry the white solid to give 5.05 g (91%) of the desired material.
後処理
- extractionExtract the mixture with ethyl acetate
- washwash twice with water
- filtrationFilter the resulting white solid
- washwash the solid with ethyl acetate
- customDry the white solid
出典と根拠
- ORDレコード
- ord-0b75bd7791a246c08b3d3c0d8087ad7c
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08049013B2
反応ノート
読み込み中…