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Potassium Carbonate → HCID 22066292、化合物

HRID 496309
ノート
印刷プレビュー

反応式

HRID 496309 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH3:23])([CH3:22])[CH2:12][CH2:13][CH2:14][CH2:15][C:16]#[C:17][Si](C)(C)C)[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[CH3:10][O:9][C:7]1[CH:6]=[C:5]([C:11]([CH3:23])([CH3:22])[CH2:12][CH2:13][CH2:14][CH2:15][C:16]#[CH:17])[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 22066290[7-(3,5-Dimethoxyphenyl)-7-methyloct-1-yn-1-yl](trimethyl)silane

生成物 1

HCID 22066292HCID 22066292、化合物収率 76%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

[7-(3,5-Dimethoxyphenyl)-7-methyl-1-octynyl]trimethysilane (900 mg, 2.73 mmol) was dissolved in 3.5 mL of anhydrous methanol. Anhydrous potassium carbonate (75 mg, 0.55 mmol, 20 mol %) was added and the heterogeneous mixture was stirred at room temperature, under argon, for 24 h. The reaction mixture was diluted with water and extracted with diethyl ether. The ether extract was dried, concentrated by rotary evaporation and the residue was purified by chromatography on silica gel (5% ethyl ether-petroleum ether) to give 540 mg (76%) of the desilylated product. Anal. calcd. for C17H24O2 C, 78.42; H, 9.29.

後処理

  1. extractionextracted with diethyl ether
  2. extractionThe ether extract
  3. customwas dried
  4. concentrationconcentrated by rotary evaporation
  5. customthe residue was purified by chromatography on silica gel (5% ethyl ether-petroleum ether)

出典と根拠

ORDレコード
ord-87494f72400b459eb37933bc8d818b2e
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06943266B1

反応ノート

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