Diethyl Ether → 3-(1,3-Dioxolan-2-YL)benzophenone

HRID 2164434

반응식

HRID 2164434 반응식
[C:1]([C:9]1[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=1C=O)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO[Si](OC)(OC)[O:20][CH2:21][CH2:22][O:23][Si](OC)(OC)OC.[C:35]([O-])(O)=O.[Na+].C(OCC)C>ClCCl.FC(F)(F)S(OC[Si](C)(C)C)(=O)=O.N1C=CC=CC=1>[C:1]([C:2]1[CH:3]=[C:4]([CH:35]2[O:20][CH2:21][CH2:22][O:23]2)[CH:5]=[CH:6][CH:7]=1)(=[O:8])[C:9]1[CH:10]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

8

반응물 4

HCID 3283Diethyl EtherHCID 1611952-BenzoylbenzaldehydeHCID 516892Sodium BicarbonateHCID 13195968HCID 13195968, 화합물

생성물 1

HCID 105150883-(1,3-Dioxolan-2-YL)benzophenone

시약·촉매·용매 3

HCID 1049Pyridine촉매HCID 2760857(Trimethylsilyl)methyl Trifluoromethanesulfonate [Trimethylsilylmethylating Reagent]촉매HCID 6344Dichloromethane용매

반응 조건

온도
20 °C

실험 절차

To a stirred solution of benzoylbenzaldehyde (2 g, 10 mmol) and 1,2-bis-(trimethoxysiloxy)ethane (2.3 g, 11 mmol) in dry dichloromethane (30 cm3) under N2 at room temperature was added trimethylsilylmethyl trifluoromethanesulphonate (5 drops). After stirring at 20° C. for 48 hours, pyridine (3 drops) was added followed by saturated NaHCO3 (20 cm3) and diethyl ether (20 cm3). The resulting mixture was stirred for 30 minutes. The ethereal layer was separated off and the aqueous layer extracted twice more with diethyl ether. The combined extracts were washed with water, dried over a mixture of anhydrous Na2CO3 and anhydrous Na2SO4 (1:1) and the solvent removed in vacuo to give 2-(3-benzoylphenyl)-1,3-dioxolane, nD20 1.5890. Yield 2.2 g (91.7%).

후처리

  1. stirringThe resulting mixture was stirred for 30 minutes
  2. customThe ethereal layer was separated off
  3. extractionthe aqueous layer extracted twice more with diethyl ether
  4. washThe combined extracts were washed with water
  5. dry with materialdried over a mixture of anhydrous Na2CO3 and anhydrous Na2SO4 (1:1)
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-2ae659d81b1c46e0943d7a38d3145739
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04504491

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