(Trimethylsilyl)imidazole → HCID 57709215, 화합물

HRID 546823

반응식

HRID 546823 반응식
[CH3:1][Si:2]([CH3:9])([CH3:8])N1C=CN=C1.[Br:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]([OH:20])([CH3:19])[CH3:18])=[CH:13][CH:12]=1.C(=O)(O)[O-].[Na+]>O1CCCC1>[Br:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]([CH3:19])([O:20][Si:2]([CH3:1])([CH3:8])[CH3:9])[CH3:18])=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 28925(Trimethylsilyl)imidazoleHCID 516892Sodium BicarbonateHCID 126819202-(4-Bromophenyl)propan-2-ol

생성물 1

HCID 57709215HCID 57709215, 화합물수율 87%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

N-trimethylsilylimidazole (80.6 mL, 0.552 mol) was added to a solution of the crude 2-(4-bromo-phenyl)-propan-2-ol in tetrahydrofuran (500 mL) in a nitrogen atmosphere at room temperature, and the mixture was stirred at the same temperature overnight. The reaction mixture was poured into a saturated aqueous sodium bicarbonate solution, followed by extraction with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was distilled off under reduced pressure. The resulting residue was subjected to silica gel chromatography (n-hexane:ethyl acetate=40:1) to give the title compound as a colorless oil (125.6 g, 87% in two steps).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-8cd1086b1c9341fca47e010f3347dc7a
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935688B2

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