Lithium Hydroxide → 2-Hydroxy-2-methyl-N-(3,3,3-trifluoro-propyl)-malonamic acid

HRID 1348657노트

반응식

HRID 1348657 반응식
C([O:3][C:4](=[O:17])[C:5]([OH:16])([CH3:15])[C:6]([NH:8][CH2:9][CH2:10][C:11]([F:14])([F:13])[F:12])=[O:7])C.[OH-].[Li+]>O1CCCC1.O>[OH:16][C:5]([CH3:15])([C:6]([NH:8][CH2:9][CH2:10][C:11]([F:12])([F:13])[F:14])=[O:7])[C:4]([OH:17])=[O:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 86605291HCID 86605291, 화합물

생성물 1

HCID 210914092-Hydroxy-2-methyl-N-(3,3,3-trifluoro-propyl)-malonamic acid수율 81%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2.30 g (7.87 mmol) 2-hydroxy-2-methyl-N-(3,3,3-trifluoro-propyl)-malonamic acid ethyl ester in 40 ml of tetrahydrofurane were added 0.33 g (7.87 mmol) of lithium hydroxide in 20 ml of water and the mixture was stirred overnight at room temperature. After concentration in vacuo water (50 ml) was added and the mixture was acidified to pH 1. Extraction with ethylacetate gave 1.46 g (81%) of the title compound as a solid, MS m/e (%): 228.1 (M−H, 100).

후처리

  1. concentrationAfter concentration in vacuo water (50 ml)
  2. additionwas added
  3. extractionExtraction with ethylacetate

출처 및 근거

ORD 기록
ord-6597474e92504327b3675aec5733b99e
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211573B2

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