Tetrabutylammonium Fluoride → 1-(4-hydroxymethyl-1-(2-trimethylsilylethoxymethyl)-1H-imidazol-2-yl)ethanone

HRID 2273305

반응식

HRID 2273305 반응식
[Si]([O:18][CH2:19][C:20]1[N:21]=[C:22]([C:33](=[O:35])[CH3:34])[N:23]([CH2:25][O:26][CH2:27][CH2:28][Si:29]([CH3:32])([CH3:31])[CH3:30])[CH:24]=1)(C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[OH:18][CH2:19][C:20]1[N:21]=[C:22]([C:33](=[O:35])[CH3:34])[N:23]([CH2:25][O:26][CH2:27][CH2:28][Si:29]([CH3:30])([CH3:32])[CH3:31])[CH:24]=1

참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium Fluoride2회HCID 71087685HCID 71087685, 화합물

생성물 1

HCID 710869721-(4-hydroxymethyl-1-(2-trimethylsilylethoxymethyl)-1H-imidazol-2-yl)ethanone수율 108.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The compound obtained in (2) (24.4 g) was dissolved in THF (200 mL), tetrabutylammonium fluoride (hereinafter sometimes referred to as TBAF) (a 1.0 M THF solution, 62.7 mL) was added under stirring, and stirring was continued for 1 hour. The reaction solution was concentrated under reduced pressure, and the resulting residue was purified by flash chromatography (ethyl acetate/hexane=25%→100%) using an amino column (trade name: Hi-Flash Column 5L Amino, manufactured by Yamazen Corporation) to give the title compound (14.1 g).

후처리

  1. additionwas added
  2. stirringstirring
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. customthe resulting residue was purified by flash chromatography (ethyl acetate/hexane=25%→100%)

출처 및 근거

ORD 기록
ord-be9491f77dfe4d37ad5c878abb97daf5
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09120835B2

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