多聚甲醛 → 3-Cyclohexylprop-2-yn-1-ol

HRID 1497

反应方程式

HRID 1497 反应方程式
[CH:1]1([C:7]#[CH:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:9]=[O:10]>CCOCC>[CH:1]1([C:7]#[C:8][CH2:9][OH:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参与物

4

反应物 2

HCID 712多聚甲醛2 次HCID 70263环己乙炔

产物 1

HCID 3166013-Cyclohexylprop-2-yn-1-ol

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂2 次

实验过程

To a solution of ethyl magesium bromide (prepared from 2.5 g of magnesium turning and 11.3 g of bromoethane) in ether was added dropwise a solution of 10.2 g of cyclohexylacetylene in ether and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled to ambient temperature and anhydrous formaldehyde (prepared from the thermal decomposition of 50 g of paraformaldehyde for 20 minutes) was bubbled into the mixture. After cooling, the reaction was quenched with saturated ammonium chloride and extracted with ether (2×100 ml). The combined ether extracts were washed with brine, dried over magnesium sulfate and evaporated to yield the product which was distilled under high vacuum at 68°-74° C. to yield 6.4 g as a colorless liquid.

后处理

  1. temperaturethe reaction mixture was refluxed for 2 hours
  2. customwas bubbled into the mixture
  3. temperatureAfter cooling
  4. customthe reaction was quenched with saturated ammonium chloride
  5. extractionextracted with ether (2×100 ml)
  6. washThe combined ether extracts were washed with brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated
  9. customto yield the product which
  10. distillationwas distilled under high vacuum at 68°-74° C.
  11. customto yield 6.4 g as a colorless liquid

来源与证据

ORD记录
ord-1df241b7ff954c60ae215c613fabf759
来源数据集
uspto-grants-1998_03
专利号
US05726162

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