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

HRID 225358ノート

反応式

HRID 225358 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 24813Phosphorus oxychloride触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8780e8d28d93486494bc8f93693a19c5
出典データセット
uspto-grants-1980_11
特許番号
US04236027

反応ノート

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