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

HRID 1372934노트

반응식

HRID 1372934 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1f054652294840449f82e344472d5240
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160875B2

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