Nitric Acid → 2-Chloro-4-fluoro-5-nitrophenyl methanesulfonate

HRID 580273

반응식

HRID 580273 반응식
S(=O)(=O)(O)O.[CH3:6][S:7]([O:10][C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[Cl:18])(=[O:9])=[O:8].[N+:19]([O-])([OH:21])=[O:20]>>[CH3:6][S:7]([O:10][C:11]1[CH:16]=[C:15]([N+:19]([O-:21])=[O:20])[C:14]([F:17])=[CH:13][C:12]=1[Cl:18])(=[O:8])=[O:9]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 98374312-Chloro-4-fluorophenyl methanesulfonate

생성물 1

HCID 137982292-Chloro-4-fluoro-5-nitrophenyl methanesulfonate수율 95.9%

실험 절차

A 95% sulfuric acid (35 ml) was added to 2-chloro-4-fluorophenyl methanesulfonate (22.5 g), to which was then added dropwise a mixture of 95% sulfuric acid (7.5 ml) and 61% nitric acid (10.3 g) under ice-water cooling and stirring to effect nitration reaction. After the completion of the addition, the reaction mixture was stirred for further 30 minutes at room temperature and then poured onto ice pieces and extracted with toluene. The toluene extract as separated was washed with 1N aqueous sodium hydroxide solution and then with water and dried over anhydrous sodium sulfate. The toluene was distilled off to afford the titled compound (25.9 g) as pale yellow crystals with melting point 64°-65.5° C.

후처리

  1. additionwas then added dropwise
  2. customreaction
  3. additionAfter the completion of the addition
  4. stirringthe reaction mixture was stirred for further 30 minutes at room temperature
  5. additionpoured onto ice pieces
  6. extractionextracted with toluene
  7. extractionThe toluene extract
  8. customas separated
  9. washwas washed with 1N aqueous sodium hydroxide solution
  10. dry with materialwith water and dried over anhydrous sodium sulfate
  11. distillationThe toluene was distilled off

출처 및 근거

ORD 기록
ord-ed88b5841c9947eabc9955a0a6407a18
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752326

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