Lithium Hydroxide → N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid

HRID 2223242ノート

反応式

HRID 2223242 の反応式
C([O:3][C:4](=[O:19])[CH:5]([CH3:18])[C:6]([NH:8][CH2:9][C:10]1[CH:15]=[C:14]([F:16])[CH:13]=[C:12]([F:17])[CH:11]=1)=[O:7])C.[OH-].[Li+]>C(O)C.O>[F:16][C:14]1[CH:15]=[C:10]([CH:11]=[C:12]([F:17])[CH:13]=1)[CH2:9][NH:8][C:6](=[O:7])[CH:5]([CH3:18])[C:4]([OH:19])=[O:3]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 69280082N-(3,5-Difluoro-benzyl)-2-methyl-malonamic acid ethyl ester

生成物 1

HCID 21091473N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of 4.0 g (14.75 mmol) N-(3,5-difluoro-benzyl)-2-methyl-malonamic acid ethyl ester in 300 ml of ethanol, 15 ml of water and 1.41 g (59 mmol) of lithium hydroxide were added and the mixture was refluxed for 5 hours. 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).

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. concentrationAfter concentration in vacuo water (50 ml)
  3. additionwas added
  4. extractionthe mixture was extracted with dichloromethane (three times 30 ml)
  5. extractionextracted with dichloromethane (four times 30 ml)

出典と根拠

ORDレコード
ord-45e91b0a0d784d0c84933259972d1081
出典データセット
uspto-grants-2008_05
特許番号
US07375099B2

反応ノート

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