Hydrochloric Acid → 5-Ethynylthiophene-2-carboxylic acid
反応式
C[Si](C)(C)[C:3]#[C:4][C:5]1[S:9][C:8]([C:10]([O:12]CC)=[O:11])=[CH:7][CH:6]=1.[Li+].[OH-].O.Cl>C1COCC1>[C:4]([C:5]1[S:9][C:8]([C:10]([OH:12])=[O:11])=[CH:7][CH:6]=1)#[CH:3]参加物
6
反応条件
- 温度
- 40 °C
実験手順
To a solution of ethyl 5-(2-trimethylsilyl-ethyn-1-yl)-thiophene-2-carboxylate prepared above (529 mg, 2.10 mmol) in THF (20 mL), 1N aq. LiOH (7.0 mL, 7.0 mmol) was added. After the mixture was stirred at 40° C. overnight, it was poured into water. The aqueous solution was acidified with 1N HCl to pH 1. The product was extracted with EtOAc. The EtOAc solution was washed with brine, dried over MgSO4, concentrated in vacuo to give 5-ethynyl-thiophene-2-carboxylic acid (316 mg). MS 153 (M+H).
後処理
- extractionThe product was extracted with EtOAc
- washThe EtOAc solution was washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-1789bd11ccc043959952d6eb129935da
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063077B2
反応ノート
読み込み中…