Potassium Hydroxide → HCID 13537979、化合物

HRID 1731273ノート

反応式

HRID 1731273 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=2[Cl:22])[C:10]=1[C:11]([F:14])([F:13])[F:12])=[O:5])C.[OH-].[K+]>C(O)C>[F:14][C:11]([F:12])([F:13])[C:10]1[N:9]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=2[Cl:22])[N:8]=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 13537978Ethyl 1-(2,4-dichlorophenyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 13537979HCID 13537979、化合物収率 62.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5-(Trifluoromethyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-4-carboxylic acid ethyl ester (3.31 grams, 0.0094 mole) and potassium hydroxide (0.8 gram, 0.014 mole) were combined in 25 ml. of ethanol. The reaction mixture was refluxed for 2 hours, then poured into 150 ml. of ice/water and filtered to remove solids. The remaining solution was acidified with concentrated HCl, filtered to separate the precipitate which was then dried and recrystallized from cyclohexane/toluene with charcoal, yielding 1.90 grams of 5-(trifluoromethyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-4-carboxylic acid, mp=154°-155° C.

後処理

  1. temperatureThe reaction mixture was refluxed for 2 hours
  2. additionpoured into 150 ml
  3. filtrationof ice/water and filtered
  4. customto remove solids
  5. filtrationfiltered
  6. customto separate the precipitate which
  7. customwas then dried
  8. customrecrystallized from cyclohexane/toluene with charcoal

出典と根拠

ORDレコード
ord-14355b1897824fe08c98ee395197e24b
出典データセット
uspto-grants-1986_11
特許番号
US04620865

反応ノート

読み込み中…