Imidazole → 1-Ethynyl-1-triethylsiloxycyclopentane

HRID 2416151

反応式

HRID 2416151 の反応式
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]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 13819ChlorotriethylsilaneHCID 870741-Ethynylcyclopentanol

生成物 1

HCID 226391411-Ethynyl-1-triethylsiloxycyclopentane収率 83.4%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-508373607b424baa800aadb00ec4ec19
出典データセット
uspto-grants-2004_11
特許番号
US06822112B1

関連ノート

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