Thiophenol → HCID 178526127、化合物

HRID 621635

反応式

HRID 621635 の反応式
[OH-:1].[K+].[C:3]1([SH:9])[CH:8]=[CH:7][CH:6]=CC=1.Br[C:11]1[CH:19]=[CH:18][C:14]([C:15](O)=O)=[CH:13][CH:12]=1.CN(C)[C:22](=O)[CH3:23]>>[C:14]1([C:15]2[CH:6]=[CH:7][C:8]([C:3]([OH:1])=[S:9])=[CH:23][CH:22]=2)[CH:18]=[CH:19][CH:11]=[CH:12][CH:13]=1

参加物

5

反応物 4

HCID 7969ThiophenolHCID 114644-Bromobenzoic acidHCID 14797Potassium HydroxideHCID 31374Dimethylacetamide

生成物 1

HCID 178526127HCID 178526127、化合物

実験手順

A solution of potassium hydroxide (20.86 g) in N,N-dimethylacetamide (70 ml) is heated to 150° C., and thereto are added with stirring thiophenol (19.52 ml) and 4-bromobenzoic acid (25.47 g) under nitrogen atmosphere at the same temperature. The mixture is refluxed under nitrogen atmosphere for 20 hours. The reaction mixture is poured into ice water (400 ml), and the mixture is washed with benzene (400 ml), and the aqueous layer is separated. The benzene layer is further extracted with 2.5N sodium hydroxide solution (100 ml×4). The extracts are combined with the above aqueous layer and adjusted to pH 1-2 with conc hydrochloric acid. The resulting precipitate is separated by filtration, washed with water and dried to give 4-phenylthiobenzoic acid (26.29 g).

後処理

  1. temperatureThe mixture is refluxed under nitrogen atmosphere for 20 hours
  2. washthe mixture is washed with benzene (400 ml)
  3. customthe aqueous layer is separated
  4. extractionThe benzene layer is further extracted with 2.5N sodium hydroxide solution (100 ml×4)
  5. customThe resulting precipitate is separated by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-1da58be216f4485eb0b7fc8eecf358ac
出典データセット
uspto-grants-1989_04
特許番号
US04824834

関連ノート

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