Benzaldehyde → T5637827

HRID 331259노트

반응식

HRID 331259 반응식
[OH-].[Na+].[OH:3][C:4]1[CH:5]=[C:6]([C:10](=[O:12])[CH3:11])[CH:7]=[CH:8][CH:9]=1.[CH:13](=O)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CCO>[OH:3][C:4]1[CH:5]=[C:6]([C:10](=[O:12])/[CH:11]=[CH:13]/[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:7]=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 84873-HydroxyacetophenoneHCID 14798Sodium Hydroxide

생성물 1

HCID 5356382T5637827수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
10 °C

실험 절차

A 250 mL round-bottomed flask was charged sequentially aq. NaOH solution (NaOH 7.1 g/H2O 50 mL) and EtOH (40 mL). The solution was maintained below 10° C. in an ice bath. 1-(3-hydroxyphenyl)ethanone (20.0 g, 147 mmol) was added and stirred for 30 min at 10° C. To the resulting mixture was then added benzaldehyde (15 mL, 1.0 eq). After being stirred for additional 1 h at 10° C., the reaction mixture was stirred at room temperature for further 26 h. The solution was concentrated by rotary evaporation under reduced pressure. The residue was dissolved in EtOAc. The organic layer was washed with 3N HCl and H2O, dried over MgSO4, and concentrated in vacuo to obtain the desired product (32.5 g, 98%).

후처리

  1. temperatureThe solution was maintained below 10° C. in an ice bath
  2. stirringAfter being stirred for additional 1 h at 10° C.
  3. stirringthe reaction mixture was stirred at room temperature for further 26 h
  4. concentrationThe solution was concentrated by rotary evaporation under reduced pressure
  5. dissolutionThe residue was dissolved in EtOAc
  6. washThe organic layer was washed with 3N HCl and H2O
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b29e8f2f974d49dc81c4aea49cd65a8c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877747B2

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