Hydrochloric Acid → 2-(4'-Ethoxy-2,2',3,3'-tetrafluorobiphenyl-4-yl)acetoaldehyde

HRID 1941722노트

반응식

HRID 1941722 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH:16]=[CH:17][O:18]C)=[C:12]([F:20])[C:11]=2[F:21])=[C:6]([F:22])[C:5]=1[F:23])[CH3:2].Cl.O>CC(C)=O>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][CH:17]=[O:18])=[C:12]([F:20])[C:11]=2[F:21])=[C:6]([F:22])[C:5]=1[F:23])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 679922734-Ethoxy-2,2',3,3'-tetrafluoro-4'-(2-methoxyvinyl)biphenyl

생성물 1

HCID 866599312-(4'-Ethoxy-2,2',3,3'-tetrafluorobiphenyl-4-yl)acetoaldehyde수율 97.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

4-Ethoxy-2,2′,3,3′-tetrafluoro-4′-(2-methoxyvinyl)biphenyl (8) (18.5 g) prepared in the sixth step was dissolved in acetone (200 ml) and hydrochloric acid (6M; 200 ml) was added, and the stirring was continued at room temperature for 1 hour. Water (200 ml) was added, and the water layer was extracted with toluene (100 ml) three times. The combined organic layer was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to leave 2-(4′-ethoxy-2,2′,3,3′-tetrafluorobiphenyl-4-yl)acetoaldehyde (9) (17.2 g) in 97.2% yield.

후처리

  1. extractionthe water layer was extracted with toluene (100 ml) three times
  2. washThe combined organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-dcdde2e59fe347179fad14f9964efd49
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389073B2

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