Propargyl bromide → HCID 22482834、化合物

HRID 751550

反応式

HRID 751550 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:12])[CH2:10][CH3:11].Br[CH2:14][C:15]#[CH:16].C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:16][C:15]#[CH:14])[CH:5]=[CH:4][C:3]=1[C:9](=[O:12])[CH2:10][CH3:11]

参加物

5

反応物 3

HCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 798562',4'-Dihydroxypropiophenone

生成物 1

HCID 22482834HCID 22482834、化合物収率 85.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2′,4′-dihydroxy-propiophenone (24.9 g, 0.15 mol), 3-bromo-propyne (24.2 g, 0.20 mol) and K2CO3 (20.7 g, 0.15 mol) in acetone (500 mL) was refluxed for 12 h. The reaction mixture was allowed assume room temperature and the precipitate was removed by filtration. The filtrate was concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 0→2% MeOH in H2O), to give 26.2 g (85%) of 1-(2-hydroxy-4-prop-2-ynyloxy-phenyl)-propan-1-one.

後処理

  1. temperaturewas refluxed for 12 h
  2. customwas allowed assume room temperature
  3. customthe precipitate was removed by filtration
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe crude product was purified by column chromatography (silica gel, 0→2% MeOH in H2O)

出典と根拠

ORDレコード
ord-fc2e97cf57644467a7a59f78d610d2b2
出典データセット
uspto-grants-2008_07
特許番号
US07405310B2

関連ノート

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