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

HRID 2223242노트

반응식

HRID 2223242 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-45e91b0a0d784d0c84933259972d1081
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07375099B2

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