Lithium Hydroxide → 2-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid

HRID 1372934ノート

反応式

HRID 1372934 の反応式
C([O:3][C:4](=[O:15])[CH:5]([CH3:14])[C:6]([NH:8][CH2:9][C:10]([F:13])([F:12])[F:11])=[O:7])C.[OH-].[Li+]>O1CCCC1.O>[CH3:14][CH:5]([C:6]([NH:8][CH2:9][C:10]([F:11])([F:12])[F:13])=[O:7])[C:4]([OH:15])=[O:3]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 867603532-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid ethyl ester

生成物 1

HCID 210724962-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid収率 84%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1.48 g (6.52 mmol) 2-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid ethyl ester in 40 ml of tetrahydrofurane, 20 ml of water and 1.09 g (26 mmol) of lithium hydroxide were added and the mixture was stirred overnight at room temperature. After concentration in vacuo water (50 ml) was added and the mixture was extracted with dichloromethane (three times 30 ml). The aqueous phase was acidified with 8 N hydrochloric acid and extracted with dichloromethane (four times 30 ml). The combined organic layers from the second extraction were dried (MgSO4) and evaporated in vacuo to give 1.09 g (84%) of the title compound as a white solid.

後処理

  1. concentrationAfter concentration in vacuo water (50 ml)
  2. additionwas added
  3. extractionthe mixture was extracted with dichloromethane (three times 30 ml)
  4. extractionextracted with dichloromethane (four times 30 ml)
  5. extractionThe combined organic layers from the second extraction
  6. dry with materialwere dried (MgSO4)
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-1f054652294840449f82e344472d5240
出典データセット
uspto-grants-2007_01
特許番号
US07160875B2

反応ノート

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