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

HRID 1823212

반응식

HRID 1823212 반응식
[F-].[K+].[N+:3]([C:6]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:7]=1Cl)([O-:5])=[O:4].[SH:16][CH2:17][CH2:18][OH:19].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:3]([C:6]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:7]=1[S:16][CH2:17][CH2:18][OH:19])([O-:5])=[O:4]

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

217 parts of potassium fluoride are introduced into a solution of 500 parts of 2,4-dinitro-1-chlorobenzene in 590 parts of N,N-dimethylformamide (DMF) and the reaction mixture is stirred for 5 hours at room temperature. 350 parts of 2-mercaptoethanol are then added dropwise, whereupon the internal temperature rises to from 60 to 65° C., and stirring is then carried out for about 15 hours at that temperature. Then, any starting materials still present are made to react by adding 34 parts of potassium carbonate. Finally, the mixture is left to cool to room temperature, salts are filtered off and the filtrate is concentrated. The oily crude product is discharged onto water, whereupon a yellow crystalline precipitate separates out. After filtering off under suction, washing and drying, 2-[2,4-dinitrophenylsulfanyl]ethanol is obtained in an almost quantitative yield and high purity.

후처리

  1. customrises to from 60 to 65° C.
  2. stirringstirring
  3. waitis then carried out for about 15 hours at that temperature
  4. customto react
  5. waitFinally, the mixture is left
  6. temperatureto cool to room temperature
  7. filtrationsalts are filtered off
  8. concentrationthe filtrate is concentrated
  9. filtrationAfter filtering off under suction
  10. washwashing
  11. customdrying

출처 및 근거

ORD 기록
ord-dd982d2c7c574d2c893625c10d8252f6
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07038024B2

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