ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → 2-Fluoro-4-chloro-5-methylsulfonyloxyphenylhydrazine

HRID 580275
ノート
印刷プレビュー

反応式

HRID 580275 の反応式
[CH3:1][S:2]([O:5][C:6]1[CH:11]=[C:10]([NH2:12])[C:9]([F:13])=[CH:8][C:7]=1[Cl:14])(=[O:4])=[O:3].Cl.[N:16]([O-])=O.[Na+].[OH-].[Na+]>O>[CH3:1][S:2]([O:5][C:6]1[CH:11]=[C:10]([NH:12][NH2:16])[C:9]([F:13])=[CH:8][C:7]=1[Cl:14])(=[O:3])=[O:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 14798Sodium HydroxideHCID 137982302-Chloro-4-fluoro-5-aminophenyl methanesulfonateHCID 23668193Sodium Nitrite

生成物 1

HCID 137982312-Fluoro-4-chloro-5-methylsulfonyloxyphenylhydrazine収率 85.9%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒
3 回

反応条件

温度
60 °C

実験手順

A mixture of 2-chloro-4-fluoro-5-aminophenyl methanesulfonate (24.0 g), 35% hydrochloric acid (63 g) and water (48 ml) was stirred at 60° C. for 30 minutes. Then, a solution of sodium nitrite (9.1 g) in water (55 ml) was added dropwise to the resulting mixture at -20° C. to effect diazotization reaction. The resulting mixture was added under stirring to a preformed and cooled (-20° C.) solution of 35% hydrochloric acid (52 ml) and stannous chloride hydrate (58 g) in water (100 ml) and the stirring was continued for 30 minutes under cooling. Then, the reaction solution was brought to room temperature and the pH of the solution was adjusted to 8.0 with an aqueous sodium hydroxide solution. Then, the reaction solution was extracted with toluene and tetrahydrofuran and the extract was washed with water, dried over anhydrous sodium sulfate and subjected to distillation under a reduced pressure to remove the solvent used, affording the titled compound (21.9 g) of the formula: ##STR54## as yellow crystals. Recrystallization from cyclohexane gave pale yellow crystals having melting point 75°-77° C.

後処理

  1. customdiazotization reaction
  2. additionThe resulting mixture was added
  3. stirringunder stirring to a preformed and
  4. waitthe stirring was continued for 30 minutes
  5. temperatureunder cooling
  6. customwas brought to room temperature
  7. extractionThen, the reaction solution was extracted with toluene and tetrahydrofuran
  8. washthe extract was washed with water
  9. dry with materialdried over anhydrous sodium sulfate
  10. distillationsubjected to distillation under a reduced pressure
  11. customto remove the solvent

出典と根拠

ORDレコード
ord-e3d7e01adb794fddb9191a26772d0467
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04752326

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート