Acetylene → 1,1-Dimethoxy-oct-7-yne
反応式
[CH3:1][O:2][CH:3]([O:10][CH3:11])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]I.[CH:12]#[CH:13]>>[CH3:1][O:2][CH:3]([O:10][CH3:11])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][C:12]#[CH:13]参加物
3
実験手順
Acetylene was bubbled through ca. 300 ml of liquid ammonia while 8.1 g (0.35 atom) of sodium was added in small pieces. After the disappearance of the blue color, dimethylsulfoxide (150 ml) was added cautiously. 1,1-Dimethoxy-6-iodohexane (8.16 g; 0.3 Mole) was then added over a period of 10 min. while acetylene was bubbled through the stirred mixture. The ammonia was allowed to evaporate and was replaced with ether. When the mixture had reached 0°, dilute NH4Cl solution was added. The organic layer was separated, washed with water, dried (Na2SO4), and evaporated. Distillation of the residue gave 48.9 g (96%) of 1,1-dimethoxy-oct-7-yne, b.p. 91°/8 Torr.
後処理
- customAcetylene was bubbled through ca. 300 ml of liquid ammonia while 8.1 g (0.35 atom) of sodium
- additionwas added in small pieces
- additionAfter the disappearance of the blue color, dimethylsulfoxide (150 ml) was added cautiously
- customwas bubbled through the stirred mixture
- customto evaporate
- customhad reached 0°
- additiondilute NH4Cl solution was added
- customThe organic layer was separated
- washwashed with water
- dry with materialdried (Na2SO4)
- customevaporated
- distillationDistillation of the residue
出典と根拠
- ORDレコード
- ord-4565cebe301f4b799e3edc3771241e31
- 出典データセット
- uspto-grants-1982_08
- 特許番号
- US04346023
反応ノート
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