Water → Ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate

HRID 850065ノート

反応式

HRID 850065 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([N:11]2[CH:15]=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:13]=[N:12]2)[CH:6]=[CH:7][C:8]=1[O:9]C)#[N:2].[Cl-].[Al+3].[Cl-].[Cl-].O>ClC(Cl)C>[C:1]([C:3]1[CH:4]=[C:5]([N:11]2[CH:15]=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:13]=[N:12]2)[CH:6]=[CH:7][C:8]=1[OH:9])#[N:2]

参加物

5

反応物 3

HCID 962WaterHCID 6451240Aluminum(III) ChlorideHCID 19366041Ethyl 1-(3-cyano-4-methoxyphenyl)pyrazole-4-carboxylate

生成物 1

HCID 15407383Ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate収率 84.7%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

反応条件

温度
70 °C

実験手順

To a solution (280 ml) of ethyl 1-(3-cyano-4-methoxyphenyl)pyrazole-4-carboxylate (28 g) in dichloroethane was added aluminum chloride (47.6 g with stirring, and the mixture was heated at 70° C. for 4 hours. After the completion of the reaction, the reaction mixture was poured into water, extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was recrystallized from ethyl acetate to give 22.5 g of ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate, melting point 233-234° C. ##STR19##

後処理

  1. customAfter the completion of the reaction
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-a4eebd45252244e5891ad6b4c86300ff
出典データセット
uspto-grants-2000_01
特許番号
US06015829

反応ノート

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