Lithium Hydroxide → 2-Fluoro-3-(2-oxopyrrolidin-1-yl)-5-trifluoromethyl Benzoic Acid

HRID 1612444ノート

反応式

HRID 1612444 の反応式
C[O:2][C:3](=[O:21])[C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[C:6]([N:14]2[CH2:18][CH2:17][CH2:16][C:15]2=[O:19])[C:5]=1[F:20].[Li+].[OH-]>O1CCOCC1>[F:20][C:5]1[C:6]([N:14]2[CH2:18][CH2:17][CH2:16][C:15]2=[O:19])=[CH:7][C:8]([C:10]([F:13])([F:11])[F:12])=[CH:9][C:4]=1[C:3]([OH:21])=[O:2]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 695896852-Fluoro-3-(2-oxopyrrolidin-1-yl)-5-trifluoromethylbenzoic Acid Methyl Ester

生成物 1

HCID 222530252-Fluoro-3-(2-oxopyrrolidin-1-yl)-5-trifluoromethyl Benzoic Acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2-Fluoro-3-(2-oxopyrrolidin-1-yl)-5-trifluoromethylbenzoic acid methyl ester (D24) in dioxane (10 ml) was treated with 1M LiOH solution (1.75 ml) and stirred at room temperature for 2 h. The dioxane was then removed under vacuum and dil. NaHCO3 and ethyl acetate were added. The aqueous phase was separated, washed with ethyl acetate, acidified with 1M HCl and extracted with ethyl acetate. The organic extract was washed with brine, dried over MgSO4 and evaporated to dryness to afford the title compound

後処理

  1. customThe dioxane was then removed under vacuum and dil. NaHCO3 and ethyl acetate
  2. additionwere added
  3. customThe aqueous phase was separated
  4. washwashed with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. extractionThe organic extract
  7. washwas washed with brine
  8. dry with materialdried over MgSO4
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-87dd4952d83e465f8382db3c1073ad8f
出典データセット
uspto-grants-2006_01
特許番号
US06992103B2

反応ノート

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