乙炔 → 1-Chloro-trans-1-octen-3-one

HRID 66997

反应方程式

HRID 66997 反应方程式
[Cl-:1].[Al+3].[Cl-].[Cl-].[CH:5]#[CH:6].[C:7](Cl)(=[O:13])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]>C(Cl)(Cl)(Cl)Cl>[Cl:1]/[CH:5]=[CH:6]/[C:7](=[O:13])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参与物

5

反应物 3

HCID 6326乙炔HCID 67340己酰氯HCID 6451240三氯化铝

产物 1

HCID 110410031-Chloro-trans-1-octen-3-one

试剂、催化剂与溶剂 1

HCID 5943四氯化碳溶剂

实验过程

To a slurry of 233.5 g. (1.75 moles) of aluminum chloride in 390 ml. of carbon tetrachloride, saturated with acetylene and cooled in an ice bath, is added over 20 minutes 201.9 g. (1.50 moles) of hexanoyl chloride. After the addition is complete, acetylene is bubbled into the mixture as rapidly as it is absorbed and for 1 hour after absorption becomes slow. The mixture is poured onto 1700 g. of ice and 720 ml. of saturated brine. The organic phase is separated and the aqueous phase is washed with ether. The combined organic phase and washings are washed with saturated brine, dried (Na2SO4) and evaporated. The residual oil is combined with 10 g. of hydroquinone and distilled to yield a colorless oil, b.p. 51°-52° C. (0.10 torr).

后处理

  1. additionis added over 20 minutes 201.9 g
  2. additionAfter the addition
  3. customacetylene is bubbled into the mixture as rapidly as it
  4. customis absorbed and for 1 hour
  5. customafter absorption
  6. additionThe mixture is poured onto 1700 g
  7. customThe organic phase is separated
  8. washthe aqueous phase is washed with ether
  9. washThe combined organic phase and washings are washed with saturated brine
  10. dry with materialdried (Na2SO4)
  11. customevaporated
  12. distillationof hydroquinone and distilled
  13. customto yield a colorless oil, b.p. 51°-52° C. (0.10 torr)

来源与证据

ORD记录
ord-332f2864e41a480dbb9cdb8d73153152
来源数据集
uspto-grants-1982_08
专利号
US04343949

关联笔记

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