Potassium fluoride dihydrate → HCID 86669589、化合物
反応式
[NH:1]1[CH:5]=[C:4]([C:6]([OH:14])([C:8]#[C:9][Si](C)(C)C)[CH3:7])[CH:3]=[N:2]1.O.O.[F-].[K+]>CO>[NH:1]1[CH:5]=[C:4]([C:6]([OH:14])([C:8]#[CH:9])[CH3:7])[CH:3]=[N:2]1参加物
4
反応条件
- 温度
- 50 °C
実験手順
In a 20-mL sealed tube, a suspension of 2-(1H-pyrazol-4-yl)-4-(trimethylsilyl)but-3-yn-2-ol (1.4 g, 6.72 mmol, 1.00 equiv) and potassium fluoride dihydrate (2.0 g) in methanol (10 mL) was stirred for 1.5 h at 50° C. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 20 mL of water. The resulting solution was extracted with 3×20 mL of tetrahydrofuran/ethyl acetate (2/1) and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 1 g (98%) of 2-(1H-pyrazol-4-yl)but-3-yn-2-ol as a solid.
後処理
- customIn a 20-mL sealed tube
- concentrationThe resulting mixture was concentrated under vacuum
- additionThe resulting solution was diluted with 20 mL of water
- extractionThe resulting solution was extracted with 3×20 mL of tetrahydrofuran/ethyl acetate (2/1)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum
- customThis resulted in 1 g (98%) of 2-(1H-pyrazol-4-yl)but-3-yn-2-ol as a solid
出典と根拠
- ORDレコード
- ord-ad2f5a22cb6940fabb0d809a0dc49bba
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034866B2
反応ノート
読み込み中…