1-Chloro-2,4-Dinitrobenzene → 2-(2,4-Dinitrophenylthio)ethanol

HRID 21676

반응식

HRID 21676 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1Cl)([O-:3])=[O:2].[F-].[K+].[SH:16][CH2:17][CH2:18][OH:19].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[S:16][CH2:17][CH2:18][OH:19])([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 61-Chloro-2,4-DinitrobenzeneHCID 15672-MercaptoethanolHCID 11430Potassium CarbonateHCID 522689Potassium Fluoride

생성물 1

HCID 92127792-(2,4-Dinitrophenylthio)ethanol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 500 parts of 2,4-dinitro-1-chlorobenzene in 590 parts of N,N-dimethylformamide (DMF) are added 217 parts of potassium fluoride and the reaction mixture is stirred at room temperature for 5 hours. Then 350 parts of 2-mercaptoethanol are added dropwise, the internal temperature rising to 60°-65 ° C., and the reaction mixture is subsequently stirred at that temperature for about 15 hours. Starting materials still present are then made to react by adding 34 parts of potassium carbonate. Finally the reaction mixture is allowed to cool down to room temperature, salts are filtered off, and the filtrate is concentrated. The oily crude product is discharged onto water, and a yellow, crystalline precipitate forms. Filtering off with suction, washing and drying leaves 2-[2,4-dinitrophenylsulfanyl]ethanol in almost quantitative yield and high purity.

후처리

  1. customrising to 60°-65 ° C.
  2. stirringthe reaction mixture is subsequently stirred at that temperature for about 15 hours
  3. customto react
  4. temperatureto cool down to room temperature
  5. filtrationsalts are filtered off
  6. concentrationthe filtrate is concentrated
  7. filtrationFiltering off with suction
  8. washwashing
  9. customdrying

출처 및 근거

ORD 기록
ord-ddef3247e5e94237b1ed439b014abdbe
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424405

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