Hydrochloric Acid → HCID 13798309, 화합물

HRID 580258노트

반응식

HRID 580258 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 13798309HCID 13798309, 화합물수율 91.8%

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d2a42dc8ee74778bdc0a69f6631eca3
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752326

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