Hydrochloric Acid → 3-Methoxyoct-1-yne
反応式
[CH:1]#[C:2][CH:3]([OH:9])[CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH2:10]([Li])CCC.CI.Cl>CCCCCC.C(COC)OC>[CH3:10][O:9][CH:3]([CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[C:2]#[CH:1]参加物
7
反応条件
- 温度
- 60 °C
実験手順
To an ice-cooled solution of 63 g. of 1-octyn-3-ol in 300 ml. of dimethoxyethane is added under an inert atmosphere 312 ml. of 1.6 M n-butyllithium in hexane dropwise over 1 hour. To the mixture is then added 145 g. of methyl iodide and the resulting mixture is stirred at ambient temperatures for 24 hours and then heated to 60° C. for 1 hour. The mixture is cooled and poured into cold dilute hydrochloric acid. The organic phase is separated, washed with water and saturated brine, dried (Na2SO4), and evaporated to an oil, dried (Na2SO4), and evaporated to an oil. Fractional distillation of the oil in vacuo yields the product as a colorless oil.
後処理
- additionTo the mixture is then added 145 g
- temperatureThe mixture is cooled
- customThe organic phase is separated
- washwashed with water and saturated brine
- dry with materialdried (Na2SO4)
- customevaporated to an oil
- dry with materialdried (Na2SO4)
- customevaporated to an oil
- distillationFractional distillation of the oil in vacuo
出典と根拠
- ORDレコード
- ord-6504c7c25c9643b9ad6209d42f4815a8
- 出典データセット
- uspto-grants-1982_08
- 特許番号
- US04343949
反応ノート
読み込み中…