Hydrochloric Acid → 1-(2-Fluoro-4-chloro-5-hydroxyphenyl)-3,4,5-trimethylpyrazole

HRID 580257노트

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HRID 580257 반응식
[F: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]([CH3:20])[C:16]([CH3:21])=[N:15]1.[OH-].[Na+].Cl>C(O)C>[F: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]([CH3:20])[C:16]([CH3:21])=[N:15]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 137982321-(2-Fluoro-4-chloro-5-methylsulfonyloxyphenyl)-3,4,5-trimethylpyrazole

생성물 1

HCID 137982331-(2-Fluoro-4-chloro-5-hydroxyphenyl)-3,4,5-trimethylpyrazole수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

A mixture of 1-(2-fluoro-4-chloro-5-methylsulfonyloxyphenyl)- 3,4,5-trimethylpyrazole (33.3 g), 2N aqueous sodium hydroxide (100 ml) and ethanol (50 ml) was stirred at 40° C. for 30 minutes. After cooling, the reaction mixture was acidified with aqueous hydrochloric acid and then extracted wth toluene. The toluene layer thus obtained was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent by distillation in vacuo gave the titled compound (24.2 g) as a pale yellow crystalline solid. Recrystallization of this solid from a mixture of n-hexane/ethyl acetate yielded a white crystalline solid. m.p. 158°-160° C.

후처리

  1. temperatureAfter cooling
  2. extractionextracted wth toluene
  3. customThe toluene layer thus obtained
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customRemoval of the solvent
  7. distillationby distillation in vacuo

출처 및 근거

ORD 기록
ord-f5fb9f8a334f4c218a4fce06a16ca2ff
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752326

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