Hydrochloric Acid → HCID 13821933、化合物

HRID 1731261ノート

反応式

HRID 1731261 の反応式
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([O:16]CC)=[O:15].[OH-].[K+].Cl>C(O)C>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([OH:16])=[O:15]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 13802161Ethyl 5-chloro-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 13821933HCID 13821933、化合物収率 81.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 7.8 g of 5-chloro-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylic acid, ethyl ester and 3.0 g of potassium hydroxide in 200 ml of 3A ethanol was refluxed for four hours. The solution was poured into ice water and acidified with hydrochloric acid. The aqueous acid solution was extracted with ethyl acetate. The organic phase was washed with water, dried, and concentrated under vacuum. The residue was recrystallized from ethanol to afford 5.7 g of 5-chloro-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylic acid. Yield 80%. mp=209°-211° C.

後処理

  1. temperaturewas refluxed for four hours
  2. extractionThe aqueous acid solution was extracted with ethyl acetate
  3. washThe organic phase was washed with water
  4. customdried
  5. concentrationconcentrated under vacuum
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-3ab39a67be364aada3382129e4e188ab
出典データセット
uspto-grants-1986_11
特許番号
US04620865

反応ノート

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