Hydrochloric Acid → 2-[(2-Nitrophenyl)sulfanyl]benzoic acid

HRID 1609275

반응식

HRID 1609275 반응식
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].F[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N+:18]([O-:20])=[O:19].C(=O)([O-])[O-].[K+].[K+].Cl>CN(C)C=O.O>[N+:18]([C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[S:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([OH:10])=[O:9])([O-:20])=[O:19]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 54432-Mercaptobenzoic AcidHCID 11430Potassium CarbonateHCID 738951-Fluoro-2-nitrobenzene

생성물 1

HCID 3769782-[(2-Nitrophenyl)sulfanyl]benzoic acid수율 77.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

In 300 ml of N,N-dimethylformamide were suspended 30.8 g of thiosalicylic acid, 28.2 g of 2-fluoronitrobenzene and 69.0 g of potassium carbonate, and the mixture was stirred at 100° C. for 2 hours. After cooling, water was added and acidified with hydrochloric acid and the crystals separated out therefrom were collected by filtration and washed with water. The crystals were then dissolved in ethyl acetate and the solution was dried over magnesium sulfate and filtered. The filtrate was concentrated and the crystals separated out therefrom were collected by filtration and dried to give 42.6 g of the title compound as yellow prisms, m.p. 169°-171° C.

후처리

  1. temperatureAfter cooling
  2. customthe crystals separated out
  3. filtrationtherefrom were collected by filtration
  4. washwashed with water
  5. dissolutionThe crystals were then dissolved in ethyl acetate
  6. dry with materialthe solution was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated
  9. customthe crystals separated out
  10. filtrationtherefrom were collected by filtration
  11. customdried

출처 및 근거

ORD 기록
ord-b78895024832442eaeaca2880d2021f5
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399703

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