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

HRID 580273

反応式

HRID 580273 の反応式
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]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2 回HCID 98374312-Chloro-4-fluorophenyl methanesulfonate

生成物 1

HCID 137982292-Chloro-4-fluoro-5-nitrophenyl methanesulfonate収率 95.9%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ed88b5841c9947eabc9955a0a6407a18
出典データセット
uspto-grants-1988_06
特許番号
US04752326

関連ノート

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