乙炔 → 1,1-Dimethoxy-oct-7-yne

HRID 67276

反应方程式

HRID 67276 反应方程式
[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]

参与物

3

反应物 2

HCID 6326乙炔HCID 205268401,1-Dimethoxy-6-iodohexane

产物 1

HCID 205268491,1-Dimethoxy-oct-7-yne收率 96%

实验过程

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.

后处理

  1. customAcetylene was bubbled through ca. 300 ml of liquid ammonia while 8.1 g (0.35 atom) of sodium
  2. additionwas added in small pieces
  3. additionAfter the disappearance of the blue color, dimethylsulfoxide (150 ml) was added cautiously
  4. customwas bubbled through the stirred mixture
  5. customto evaporate
  6. customhad reached 0°
  7. additiondilute NH4Cl solution was added
  8. customThe organic layer was separated
  9. washwashed with water
  10. dry with materialdried (Na2SO4)
  11. customevaporated
  12. distillationDistillation of the residue

来源与证据

ORD记录
ord-4565cebe301f4b799e3edc3771241e31
来源数据集
uspto-grants-1982_08
专利号
US04346023

关联笔记

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