Imidazole → 1-Ethynyl-1-triethylsiloxycyclopentane

HRID 2416151

반응식

HRID 2416151 반응식
CN(C)C=O.[C:6]([C:8]1([OH:13])[CH2:12][CH2:11][CH2:10][CH2:9]1)#[CH:7].N1C=CN=C1.[CH2:19]([Si:21]([CH2:25][CH3:26])([CH2:23][CH3:24])Cl)[CH3:20]>CCCCCC>[C:6]([C:8]1([O:13][Si:21]([CH2:25][CH3:26])([CH2:23][CH3:24])[CH2:19][CH3:20])[CH2:12][CH2:11][CH2:10][CH2:9]1)#[CH:7]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 13819ChlorotriethylsilaneHCID 870741-Ethynylcyclopentanol

생성물 1

HCID 226391411-Ethynyl-1-triethylsiloxycyclopentane수율 83.4%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

To a dimethylformamide solution (49.5 ml) of 1-ethynyl-1-hydroxycyclopentane (5.45 g, 49.5 mmol) were added imidazole (6.74 g, 99.0 mmol) and triethylchlorosilane (9.97 ml, 59.4 mmol) at room temperature, followed by stirring for 30 minutes. The reaction solution was added to a mixture of n-hexane and a saturated aqueous sodium bicarbonate solution, and the organic layer was separated. The aqueous layer was extracted with hexane, and the organic layers were combined, washed with a saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulfate. After filtration, the filtrate was evaporated under reduced pressure to give the title compound (9.26 g).

후처리

  1. customa saturated aqueous sodium bicarbonate solution, and the organic layer was separated
  2. extractionThe aqueous layer was extracted with hexane
  3. washwashed with a saturated aqueous sodium bicarbonate solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter filtration
  6. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-508373607b424baa800aadb00ec4ec19
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06822112B1

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