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Ethylene Glycol → HCID 68160183、化合物

HRID 1468755
ノート
印刷プレビュー

反応式

HRID 1468755 の反応式
[Si:1]([O:8][CH2:9][C:10]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:11])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[CH2:18](O)[CH2:19][OH:20]>C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:4]([Si:1]([CH3:3])([CH3:2])[O:8][CH2:9][C:10]1([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[O:20][CH2:19][CH2:18][O:11]1)([CH3:7])([CH3:6])[CH3:5]
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 174Ethylene GlycolHCID 135233382-(Tert-butyldimethylsilanyloxy)-1-phenylethanone

生成物 1

HCID 68160183HCID 68160183、化合物収率 58.4%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 241Benzene溶媒

実験手順

2-(tert-Butyldimethylsilanyloxy)-1-phenylethanone (8.0 g, 32 mmol), ethylene glycol (1.99 g, 32 mmol), and p-toluenesulfonic acid (50 mg) was suspended in benzene (50 ml). The mixture was stirred under reflux for 5 hours. The solvent was evaporated under reduced pressure. The residue was treated with water and ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The crude was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=1/1) to give tert-butyldimethyl-(2-phenyl-[1,3]dioxolan-2-yl-methoxy)silane (5.5 g, 18.7 mmol, 58%) as a yellow oil.

後処理

  1. temperatureunder reflux for 5 hours
  2. customThe solvent was evaporated under reduced pressure
  3. additionThe residue was treated with water and ethyl acetate
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe crude was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=1/1)

出典と根拠

ORDレコード
ord-93f3c35c28b84cc497ed2dee194b995a
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09006232B2

反応ノート

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