Hydrochloric Acid → 3-Methoxyoct-1-yne

HRID 436128

반응식

HRID 436128 반응식
[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]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 131661-Octyn-3-olHCID 178418339Butyllithium

생성물 1

HCID 146912763-Methoxyoct-1-yne

시약·촉매·용매 2

HCID 8058Hexane용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  1. additionTo the mixture is then added 145 g
  2. temperatureThe mixture is cooled
  3. customThe organic phase is separated
  4. washwashed with water and saturated brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated to an oil
  7. dry with materialdried (Na2SO4)
  8. customevaporated to an oil
  9. distillationFractional distillation of the oil in vacuo

출처 및 근거

ORD 기록
ord-276ba9cb640743898e5893cf61fa4438
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04007210

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