Imidazole → 3-(tert-butyldimethylsilyloxy)dihydrofuran-2(3H)-one

HRID 13382

반응식

HRID 13382 반응식
N1C=CN=C1.[Si:6](Cl)([C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:8])[CH3:7].CN(C)C=O.[OH:19][CH:20]1[CH2:24][CH2:23][O:22][C:21]1=[O:25]>C(OCC)(=O)C>[Si:6]([O:19][CH:20]1[CH2:24][CH2:23][O:22][C:21]1=[O:25])([C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:8])[CH3:7]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 545831alpha-Hydroxy-gamma-butyrolactone

생성물 1

HCID 50462413-(tert-butyldimethylsilyloxy)dihydrofuran-2(3H)-one

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

9.0 g of imidazole and 15.9 g of t-butyldimethylsilyl chloride were added in order to a dimethylformamide (180 ml) solution of 9.0 g of 3-hydroxydihydrofuran-2-(3H)-one, and the reaction liquid was stirred for 1 hour at room temperature. The reaction liquid was diluted with ethyl acetate, washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=5/1) to obtain the entitled compound as a colorless oily substance.

후처리

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=5/1)
  7. customto obtain the entitled compound as a colorless oily substance

출처 및 근거

ORD 기록
ord-231380418bd64564bb18d212d111574c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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