Ethylbenzene → 4'-Ethylbenzoin

HRID 375038

반응식

HRID 375038 반응식
O.[C:2]1([C:8]([CH:10]=[O:11])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:13]>ClC(Cl)C.[Ti](Cl)(Cl)(Cl)Cl>[CH2:12]([C:14]1[CH:19]=[CH:18][C:17]([CH:10]([OH:11])[C:8](=[O:9])[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:16][CH:15]=1)[CH3:13]

참가 물질

5

반응물 2

HCID 7500EthylbenzeneHCID 12215922Glyoxal, phenyl-, hydrate

생성물 1

HCID 153006894'-Ethylbenzoin수율 74%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 63651,1-Dichloroethane용매

실험 절차

Phenylglyoxal monohydrate (304 mg, 2 mM) and ethylbenzene (0.49 ml, 4 mM) were dissolved in dichloroethane (4 ml), titanium tetrachloride (0.33 ml, 3 mM) was added, and reacted at room temperature for 2 hours. The reaction mixture was extracted with ethylacetate, the extract was washed with saturated sodium hydrogen carbonate solution and brine, dried with sodium sulfate anhydrous, and then concentrated to obtain a yellow-colored oil. The oil was crystallized from a petroleum ether/diethylether to obtain 357.1 mg (74.0% yield) of 4'-ethylbenzoin.

후처리

  1. customreacted at room temperature for 2 hours
  2. extractionThe reaction mixture was extracted with ethylacetate
  3. washthe extract was washed with saturated sodium hydrogen carbonate solution and brine
  4. dry with materialdried with sodium sulfate anhydrous
  5. concentrationconcentrated
  6. customto obtain a yellow-colored oil
  7. customThe oil was crystallized from a petroleum ether/diethylether

출처 및 근거

ORD 기록
ord-374784cfa61e419b83146e90f4f0eb8b
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484689

연결된 노트

불러오는 중…