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

HRID 1941722ノート

反応式

HRID 1941722 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dcdde2e59fe347179fad14f9964efd49
出典データセット
uspto-grants-2013_03
特許番号
US08389073B2

反応ノート

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