3,4-dihydro-2H-pyran → 2-But-3-enoxyoxane

HRID 1582515

반응식

HRID 1582515 반응식
P(Cl)(Cl)(Cl)=O.[CH2:6]([OH:10])[C:7]#[C:8][CH3:9].[O:11]1[CH:16]=[CH:15][CH2:14][CH2:13][CH2:12]1>C(Cl)Cl>[CH2:6]([O:10][CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16][O:11]1)[CH2:7][CH:8]=[CH2:9]

참가 물질

5

반응물 3

HCID 80803,4-dihydro-2H-pyranHCID 129912-Butyn-1-olHCID 24813Phosphorus oxychloride

생성물 1

HCID 3199452-But-3-enoxyoxane

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of phosphoryl chloride (0.5 ml in 10 ml of DCM) was added with care to a solution of but-2-yn-1-ol (8.75 g, 125 mmol) and dihydropyran (10.50 g, 125 mmol) in DCM (80 ml). The reaction mixture was stirred at room temperature for 16 h, washed with sodium hydrogen carbonate solution (3 times), dried (MgSO4) and the solvent removed in vacuo to yield a colorless oil. The crude product was purified by column chromatography [silica gel, euted with hexane/ethyl acetate (4:1), Rf: 0.36] to yield a colorless oil.

후처리

  1. washwashed with sodium hydrogen carbonate solution (3 times)
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customto yield a colorless oil
  5. customThe crude product was purified by column chromatography [silica gel, euted with hexane/ethyl acetate (4:1), Rf: 0.36]
  6. customto yield a colorless oil

출처 및 근거

ORD 기록
ord-1813885332774ff78541c40e688d6bc8
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737124B2

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