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

HRID 580257ノート

反応式

HRID 580257 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f5fb9f8a334f4c218a4fce06a16ca2ff
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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