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

HRID 1348657ノート

反応式

HRID 1348657 の反応式
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]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 86605291HCID 86605291、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-6597474e92504327b3675aec5733b99e
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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