Benzene → HCID 178526127, 화합물

HRID 37148

반응식

HRID 37148 반응식
CN(C)C(=O)C.C1([SH:13])C=CC=CC=1.Br[C:15]1[CH:23]=[CH:22][C:18]([C:19]([OH:21])=O)=[CH:17][CH:16]=1.[CH:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>[OH-].[K+]>[C:24]1([C:15]2[CH:16]=[CH:17][C:18]([C:19]([OH:21])=[S:13])=[CH:22][CH:23]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 241BenzeneHCID 7969ThiophenolHCID 114644-Bromobenzoic acidHCID 31374Dimethylacetamide

생성물 1

HCID 178526127HCID 178526127, 화합물

시약·촉매·용매 1

HCID 14797Potassium Hydroxide용매

반응 조건

온도
150 °C

실험 절차

A solution of 70 ml of N,N-dimethylacetamide in which 20.86 g of potassium hydroxide was dissolved was heated to 150° C., and 19.52 ml of thiophenol and 25.47 g of 4-bromobenzoic acid were added under nitrogen atmosphere while stirring at the same temperature. After reflux for 20 hours under nitrogen atmosphere, the reaction mixture was poured into 400 ml of ice water, and 400 ml of benzene was added to wash, and the water layer was separated. The benzene layer was extracted with 2.5N sodium hydroxide (100 ml×4). The extract was combined with the water layer and the pH was adjusted to 1 to 2 with concentrated hydrochloric acid, and the precipitate was filtered, washed in water, dried, and 4-phenylthiobenzoic acid was obtained (26.29 g).

후처리

  1. temperatureAfter reflux for 20 hours under nitrogen atmosphere
  2. additionwas added
  3. washto wash
  4. customthe water layer was separated
  5. extractionThe benzene layer was extracted with 2.5N sodium hydroxide (100 ml×4)
  6. filtrationthe precipitate was filtered
  7. washwashed in water
  8. customdried

출처 및 근거

ORD 기록
ord-3b002c86051440ea974d1ecc49654d6f
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420128

연결된 노트

불러오는 중…