Lithium hydroxide, monohydrate → HCID 178524946、化合物

HRID 659797ノート

反応式

HRID 659797 の反応式
C([O:3][C:4]([C:6]1[C:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[Cl:18])=[CH:9][NH:8][N:7]=1)=[O:5])C.O.[OH-].[Li+]>C1COCC1.O>[Cl:18][C:12]1[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=1[C:10]1[C:6]([C:4]([OH:5])=[O:3])=[N:7][NH:8][CH:9]=1

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 178470487HCID 178470487、化合物

生成物 1

HCID 178524946HCID 178524946、化合物収率 108.1%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

A solution of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid ethyl ester (205 mg; 0.72 mmol) and lithium hydroxide monohydrate (125 mg; 2.9 mmol) in 1:1 THF/water (10 ml) was heated at 60° C. overnight. The THF was removed by evaporation, the aqueous phase acidified with 1M hydrochloric acid then extracted with ethyl acetate (20 ml). The ethyl acetate layer was dried (MgSO4), filtered and evaporated to give 200 mg of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid. (LC/MS: [M+H]+ 256.85).

後処理

  1. customThe THF was removed by evaporation
  2. extractionthen extracted with ethyl acetate (20 ml)
  3. dry with materialThe ethyl acetate layer was dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-81eaf89f066640fe9a3186a1daef1578
出典データセット
uspto-grants-2011_12
特許番号
US08080666B2

反応ノート

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