Thiophenol → HCID 178526127, 화합물

HRID 621635

반응식

HRID 621635 반응식
[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

참가 물질

5

반응물 4

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

생성물 1

HCID 178526127HCID 178526127, 화합물

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1da58be216f4485eb0b7fc8eecf358ac
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824834

연결된 노트

불러오는 중…