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Tetrahydrofuran → 4-Ethoxy-2,2',3,3'-tetrafluorobiphenyl-4-carboaldehyde

HRID 1941720
ノート
印刷プレビュー

反応式

HRID 1941720 の反応式
C1C[O:4][CH2:3]C1.[CH2:6]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[C:16]=2[F:22])=[C:11]([F:23])[C:10]=1[F:24])[CH3:7].C([Li])(CC)C>CN(C=O)C>[CH2:6]([O:8][C:9]1([CH:3]=[O:4])[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[C:16]=2[F:22])=[C:11]([F:23])[CH:10]1[F:24])[CH3:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 58453709HCID 58453709、化合物HCID 178418400CID 53628100

生成物 1

HCID 866599304-Ethoxy-2,2',3,3'-tetrafluorobiphenyl-4-carboaldehyde収率 70%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
-65 °C

実験手順

THF (400 ml) was added to 4-ethoxy-2,2′,3,3′-tetrafluorobiphenyl (6) (39.25 g) prepared by means of a conventional coupling reaction in a reaction vessel under an atmosphere of nitrogen. The solution was cooled to −65° C. or lower, and sec-butyllithium (1.08 M in cyclohexane and n-hexane; 141.3 ml) was added dropwise. After the reaction mixture had been stirred at −65° C. for another 1 hour, N,N,-dimethylformamide (21.2 g) was added dropwise, and the reaction mixture was warmed slowly to room temperature. The reaction mixture was quenched with a saturated aqueous solution of ammonium chloride, and water (500 ml) was added to give two layers. The water layer was extracted with toluene (200 ml) twice, and the combined organic layer was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was treated with silica gel chromatography (silica gel: 30 g, eluent: toluene) to give 4-ethoxy-2,2′,3,3′-tetrafluorobiphenyl-4-carboaldehyde (7) (30 g) in 70% yield.

後処理

  1. customprepared by means of a conventional coupling reaction in a reaction vessel under an atmosphere of nitrogen
  2. temperaturethe reaction mixture was warmed slowly to room temperature
  3. customThe reaction mixture was quenched with a saturated aqueous solution of ammonium chloride, and water (500 ml)
  4. additionwas added
  5. customto give two layers
  6. extractionThe water layer was extracted with toluene (200 ml) twice
  7. washthe combined organic layer was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationThe solvent was distilled off under reduced pressure
  10. additionThe residue was treated with silica gel chromatography (silica gel: 30 g, eluent: toluene)

出典と根拠

ORDレコード
ord-ff00ac905d7943bcaa639a49024ff2da
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08389073B2

反応ノート

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