3,4-dihydro-2H-pyran → 2-[(4,4-Dimethyloct-1-YN-3-YL)oxy]oxane

HRID 225358노트

반응식

HRID 225358 반응식
[CH3:1][C:2]([CH3:11])([CH2:7][CH2:8][CH2:9][CH3:10])[CH:3]([OH:6])[C:4]#[CH:5].[O:12]1[CH:17]=[CH:16][CH2:15][CH2:14][CH2:13]1>P(Cl)(Cl)(Cl)=O.C(N(CC)CC)C>[CH3:1][C:2]([CH3:11])([CH2:7][CH2:8][CH2:9][CH3:10])[CH:3]([O:6][CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][O:12]1)[C:4]#[CH:5]

참가 물질

5

반응물 2

HCID 80803,4-dihydro-2H-pyranHCID 145163694,4-Dimethyl-1-octyn-3-ol

생성물 1

HCID 145163702-[(4,4-Dimethyloct-1-YN-3-YL)oxy]oxane

시약·촉매·용매 2

HCID 8471Triethylamine촉매HCID 24813Phosphorus oxychloride촉매

실험 절차

To a solution of 23.1 g. (0.150 mole) of 4,4-dimethyl-1-octyn-3-ol (Example 149) in 126 g. of freshly distilled dihydropyran is added 1 drop of phosphorus oxychloride and the solution is maintained at ambient temperature in a tightly stoppered flask for 20 hours. Five drops of triethylamine are then added and the mixture is evaporated in vacuo to an oil. The oil is chromatographed on 600 g. of silica gel and the product is eluted with 5% ethyl acetate in benzene yielding a colorless oil.

후처리

  1. customthe mixture is evaporated in vacuo to an oil
  2. customThe oil is chromatographed on 600 g
  3. washof silica gel and the product is eluted with 5% ethyl acetate in benzene yielding a colorless oil

출처 및 근거

ORD 기록
ord-8780e8d28d93486494bc8f93693a19c5
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04236027

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