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

HRID 1348654노트

반응식

HRID 1348654 반응식
C([O:3][C:4](=[O:16])[C:5]([OH:15])([CH3:14])[C:6]([NH:8][CH2:9][C:10]([F:13])([F:12])[F:11])=[O:7])C.[OH-].[Li+]>O1CCCC1.O>[OH:15][C:5]([CH3:14])([C:6]([NH:8][CH2:9][C:10]([F:11])([F:12])[F:13])=[O:7])[C:4]([OH:16])=[O:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 86605290HCID 86605290, 화합물

생성물 1

HCID 210914072-Hydroxy-2-methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid수율 85%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3.60 g (15.0 mmol) (S or R)-2-hydroxy-2-methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid ethyl ester, entity A, in 50 ml of tetrahydrofurane were added 0.65 g (16 mmol) of lithium hydroxide in 25 ml of water and the mixture was stirred for 18 hours at room temperature. After removal of the organic solvent by distillation the mixture was acidified to pH 1. Extraction with ethylacetate gave 2.70 g (85%) of the title compound as an oil, MS m/e (%): 214.3 (M−H, 100).

후처리

  1. customAfter removal of the organic solvent
  2. distillationby distillation the mixture
  3. extractionExtraction with ethylacetate

출처 및 근거

ORD 기록
ord-eca943983e924e3e8e723f3f96e2d01d
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211573B2

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