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

HRID 2066390

반응식

HRID 2066390 반응식
[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]

참가 물질

6

반응물 3

HCID 84873-HydroxyacetophenoneHCID 25517Ammonium ChlorideHCID 178418573HCID 178418573, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-39c07a8b5ee34016b3b834139786b5f3
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293715B2

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