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Pyridine → 5-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-2-fluorobenzonitrile

HRID 1848309
ノート
印刷プレビュー

反応式

HRID 1848309 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9](O)([C:22]([F:25])([F:24])[F:23])[CH2:10][C:11]([C:13]2[CH:14]=[CH:15][C:16]([F:21])=[C:17]([CH:20]=2)[C:18]#[N:19])=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.S(Cl)(Cl)=O.N1C=CC=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:22]([F:25])([F:24])[F:23])=[CH:10][C:11]([C:13]2[CH:14]=[CH:15][C:16]([F:21])=[C:17]([CH:20]=2)[C:18]#[N:19])=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1
参加物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 1049PyridineHCID 24386Thionyl ChlorideHCID 866421905-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-fluorobenzonitrile

生成物 1

HCID 866421895-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-2-fluorobenzonitrile収率 85.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

After adding 5.85 g of toluene to 1.95 g (4.81 mmol) of 5-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-fluorobenzonitrile, 1.14 g (9.62 mmol) of thionyl chloride and 0.76 g (9.62 mmol) of pyridine were added at 80° C., and stirred for 2 hours. The reaction solution was cooled to room temperature, and separated by adding 20 ml of toluene and 10 ml of water. After washing the toluene phase with an aqueous solution of 0.39 g of sodium hydroxide dissolved into 10 ml of water, the phase was washed with water. The solvent was distilled off under reduced pressure to obtain 1.59 g of 5-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-2-fluorobenzonitrile (yield 85.2%).

後処理

  1. additionwere added at 80° C.
  2. customseparated
  3. additionby adding 20 ml of toluene and 10 ml of water
  4. washAfter washing the toluene phase with an aqueous solution of 0.39 g of sodium hydroxide
  5. dissolutiondissolved into 10 ml of water
  6. washthe phase was washed with water
  7. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-17ce7b9b98044bc0b36aa2cac5096454
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952175B2

反応ノート

読み込み中…

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