Hydrochloric Acid → HCID 13798309、化合物

HRID 580258ノート

反応式

HRID 580258 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]S(C)(=O)=O)=[CH:4][C:3]=1[N:14]1[C:18]([CH3:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[N:15]1.[OH-].[Na+].Cl>>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:14]1[C:18]([CH3:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[N:15]1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 137983241-(2,4-Dichloro-5-methylsulfonyloxyphenyl)-3,5-dimethyl-4-chloropyrazole

生成物 1

HCID 13798309HCID 13798309、化合物収率 91.8%

反応条件

温度
50 °C

実験手順

A mixture of 1-(2,4-dichloro-5-methylsulfonyloxyphenyl)-3,5-dimethyl-4-chloropyrazole (37.0 g) and 2N aqueous sodium hydroxide was stirred at 50° C. for 30 minutes. After cooling, the reaction mixture was acidified with aqueous hydrochloric acid and then extracted with toluene. The resulting toluene layer was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent by distillation in vacuo gave the titled compound (26.8 g) as a pale yellow crystalline solid. Recrystallization of this solid from a mixture of n-hexane/ethyl acetate afforded a white crystalline solid. m.p. 172°-174° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with toluene
  3. washThe resulting toluene layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customRemoval of the solvent
  6. distillationby distillation in vacuo

出典と根拠

ORDレコード
ord-8d2a42dc8ee74778bdc0a69f6631eca3
出典データセット
uspto-grants-1988_06
特許番号
US04752326

反応ノート

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