3-Hydroxyacetophenone → 3-(2-Hydroxypropan-2-yl)phenol

HRID 2066390

反応式

HRID 2066390 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[CH3:11][Mg]Br.[Cl-].[NH4+]>O1CCCC1.C(OCC)C>[OH:10][C:8]([C:4]1[CH:3]=[C:2]([OH:1])[CH:7]=[CH:6][CH:5]=1)([CH3:11])[CH3:9]

参加物

6

反応物 3

HCID 84873-HydroxyacetophenoneHCID 25517Ammonium ChlorideHCID 178418573HCID 178418573、化合物

生成物 1

HCID 4581423-(2-Hydroxypropan-2-yl)phenol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3′-Hydroxyacetophenone (500 mg) was dissolved in tetrahydrofuran (10 ml), and the solution was slowly added dropwise with a 3 M solution of methylmagnesium bromide in diethyl ether (3.7 ml) under ice cooling. The mixture was stirred at the same temperature for 2 hours, and then added with saturated aqueous ammonium chloride, the mixture was extracted with ethyl acetate, and the organic layer was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1 to 1:1) to obtain the title compound (224.3 mg).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. concentrationthe organic layer was concentrated under reduced pressure
  3. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1 to 1:1)

出典と根拠

ORDレコード
ord-39c07a8b5ee34016b3b834139786b5f3
出典データセット
uspto-grants-2012_10
特許番号
US08293715B2

関連ノート

読み込み中…