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Ethylene Glycol → HCID 68160183, 화합물

HRID 1468755
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HRID 1468755 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 174Ethylene GlycolHCID 135233382-(Tert-butyldimethylsilanyloxy)-1-phenylethanone

생성물 1

HCID 68160183HCID 68160183, 화합물수율 58.4%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 241Benzene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-93f3c35c28b84cc497ed2dee194b995a
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006232B2

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