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

HRID 1348654ノート

反応式

HRID 1348654 の反応式
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]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 86605290HCID 86605290、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-eca943983e924e3e8e723f3f96e2d01d
出典データセット
uspto-grants-2007_05
特許番号
US07211573B2

反応ノート

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