Hydrochloric Acid → 3-Methoxyoct-1-yne

HRID 1112712

반응식

HRID 1112712 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

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 treated 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. additiontreated to 60° C. for 1 hour
  3. temperatureThe mixture is cooled
  4. customThe organic phase is separated
  5. washwashed with water and saturated brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated to an oil
  8. dry with materialdried (Na2SO4)
  9. customevaporated to an oil
  10. distillationFractional distillation of the oil in vacuo

출처 및 근거

ORD 기록
ord-a3cf842bc7dc4fcfa2b08270a2c3e423
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04123456

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