Water → 1-Ethynyl-3,5-dimethylbenzene
反応式
C[Si](C)(C)[C:3]#[C:4][C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([CH3:12])[CH:6]=1.[OH-].[K+].O>C1COCC1.CO>[CH3:12][C:7]1[CH:6]=[C:5]([C:4]#[CH:3])[CH:10]=[C:9]([CH3:11])[CH:8]=1参加物
6
実験手順
A solution of crude 1-trimethylsilyl-2-(3,5-dimethylphenyl)acetylene (105 mmol, theoretical maximum) in THF (70 mL) and MeOH (280 mL) was cooled in an ice/water bath during addition of 8N KOH (16 mL, 128 mmol) and water (25 mL) and the reaction was then removed from ice/water bath. After 1 h, approximately half of the organic solvent was removed in vacuo. Hexanes (1 L) and water (400 mL) were added. The organic layer was washed with saturated brine, dried (Na2SO4), and concentrated to give 11.3 g of 1-(3,5-dimethylphenyl)acetylene as a brown oil:
後処理
- customthe reaction was then removed from ice/water bath
- customapproximately half of the organic solvent was removed in vacuo
- additionHexanes (1 L) and water (400 mL) were added
- washThe organic layer was washed with saturated brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f2b51390df4e4b91ab52cc34b220a5d7
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06310247B1
反応ノート
読み込み中…