1,2-Dichloro-1-fluoroethane → 2-(2-Chloro-2-fluoroethylthio)-phenylsulfonamide

HRID 374352

반응식

HRID 374352 반응식
C(N(CC)CC)C.[SH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[S:15]([NH2:18])(=[O:17])=[O:16].[Cl:19][CH:20]([F:23])[CH2:21]Cl>CO>[Cl:19][CH:20]([F:23])[CH2:21][S:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[S:15]([NH2:18])(=[O:17])=[O:16]

참가 물질

4

반응물 2

HCID 790041,2-Dichloro-1-fluoroethaneHCID 198097532-Mercaptophenylsulfonamide triethylamine salt

생성물 1

HCID 190867512-(2-Chloro-2-fluoroethylthio)-phenylsulfonamide수율 49.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 217.8 g of the 2-mercaptophenylsulfonamide triethylamine salt obtained in accordance with Example H6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred for 24 hours at a temperature of +65° C. to +70° C. and is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C. The reaction mixture is then evaporated and the residue is triturated with water. Extracting the mixture with ethyl acetate, washing the extract with water, drying it over sodium sulfate and evaporating it and purifying the residue by chromatography with methylene chloride gives 99.5 g (49.2% of theory) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of +88° C. to +89° C.

후처리

  1. stirringis then stirred in an autoclave for a further 24 hours at +95° C. to +100° C
  2. customThe reaction mixture is then evaporated
  3. customthe residue is triturated with water
  4. extractionExtracting the mixture with ethyl acetate
  5. washwashing the
  6. extractionextract with water
  7. dry with materialdrying it over sodium sulfate
  8. customevaporating it
  9. custompurifying the residue by chromatography with methylene chloride

출처 및 근거

ORD 기록
ord-f06dd4e54b284f768e15c50d816a7db2
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166430

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