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Boron trifluoride etherate → 5-Hydroxy-2-methyl-5-(2-trimethylsilylfuran-4-yl)-2-pentenal

HRID 1195856
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HRID 1195856 반응식
[CH3:1][Si:2]([CH3:11])([CH3:10])[C:3]1[O:7][CH:6]=[C:5]([CH:8]=[O:9])[CH:4]=1.B(F)(F)F.CCOCC.[CH3:21][C:22]([CH:29]=[CH2:30])=[CH:23][O:24][Si](C)(C)C>C(Cl)Cl>[OH:9][CH:8]([C:5]1[CH:4]=[C:3]([Si:2]([CH3:11])([CH3:10])[CH3:1])[O:7][CH:6]=1)[CH2:30][CH:29]=[C:22]([CH3:21])[CH:23]=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8000Boron trifluoride etherateHCID 1791012-Methyl-1-trimethylsilyloxy-1,3-butadieneHCID 156632515-(Trimethylsilyl)furan-3-carbaldehyde

생성물 1

HCID 572938505-Hydroxy-2-methyl-5-(2-trimethylsilylfuran-4-yl)-2-pentenal

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 5-trimethylsilyl-3-furaldehyde (0.382 g., 2.27 mmol) in dry methylene chloride (15 ml) at -50° under argon was added dropwise boron trifloride etherate (0.28 ml, 2.3 mmol). This addition was followed by the dropwise addition of 2-methyl-1-trimethylsilyloxy-1,3-butadiene (0.356 g., 2.3 mmol). The solution was stirred at -50° to -60° for 18 hours, quenched by the addition of several ml saturated sodium bicarbonate solution, warmed to room temperature and poured into methylene chloride. The organic portion was washed once with saturated bicarbonate solution, once with water, once with saturated sodium chloride solution, dried over magnesium sulfate, filtered and concentrated to give a yellow oil which consisted of several components by TLC. The mixture was applied to a chromatography column (silica) and eluted with 30% ethyl acetate/hexane. Eluted last was the desired alcohol, which was concentrated to give a yellow gum.

후처리

  1. additionThis addition
  2. customquenched by the addition of several ml saturated sodium bicarbonate solution
  3. additionpoured into methylene chloride
  4. washThe organic portion was washed once with saturated bicarbonate solution, once with water, once with saturated sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give a yellow oil which
  9. washeluted with 30% ethyl acetate/hexane
  10. washEluted last
  11. concentrationwas concentrated
  12. customto give a yellow gum

출처 및 근거

ORD 기록
ord-69d1fe291f204e00b0a6c224f4787f3c
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05112853

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