Potassium Carbonate → 4-{[3-Chloro-5-(trifluoromethyl)phenyl]oxy}benzaldehyde

HRID 474676

반응식

HRID 474676 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:12])[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.F[C:14]1[CH:21]=[CH:20][C:17]([CH:18]=[O:19])=[CH:16][CH:15]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([O:12][C:14]2[CH:21]=[CH:20][C:17]([CH:18]=[O:19])=[CH:16][CH:15]=2)[CH:5]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:7]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 38527183-Chloro-5-hydroxybenzotrifluoride

생성물 1

HCID 866662124-{[3-Chloro-5-(trifluoromethyl)phenyl]oxy}benzaldehyde수율 108%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
130 °C

실험 절차

To a solution of 3-chloro-5-(trifluoromethyl)phenol (2 g, 10.18 mmol) and 4-fluorobenzaldehyde (1.201 ml, 11.19 mmol) in DMF (30 mL), was added K2CO3 (2.109 g, 15.26 mmol). The mixture was heated at 130° C. overnight. After cooling, the reaction mixture was diluted in water, extracted with EA. The organic phase was washed with water and brine, dried over Na2SO4, concentrated to afford the title compound (3.3 g, 10.98 mmol, 108% yield) as a brown oil. LCMS: rt=3.89 min, [M+H+]=301

후처리

  1. temperatureAfter cooling
  2. extractionextracted with EA
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-356c38f99a2b4a64b008b97cf85af072
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637536B2

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