Hydrochloric Acid → 2-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

HRID 1619964노트

반응식

HRID 1619964 반응식
[CH2:1]([N:8]1[C:12]2[CH:13]=[CH:14][C:15]([C:17](=[O:31])[CH:18]([CH:20]([C:26]([O:28]CC)=[O:27])[C:21]([O:23]CC)=[O:22])[CH3:19])=[CH:16][C:11]=2[O:10]C1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl>C(O)C>[CH2:1]([NH:8][C:12]1[CH:13]=[CH:14][C:15]([C:17](=[O:31])[CH:18]([CH:20]([C:26]([OH:28])=[O:27])[C:21]([OH:23])=[O:22])[CH3:19])=[CH:16][C:11]=1[OH:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 67466180Diethyl 2-[2-(3-benzyl-2-oxo-2,3-dihydro-benzoxazol-6-yl)-1-methyl-2-oxo-ethyl]-malonate

생성물 1

HCID 674670302-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

5 g (11.4 mmol) diethyl 2-[2-(3-benzyl-2-oxo-2,3-dihydro-benzoxazol-6-yl)-1-methyl-2-oxo-ethyl]-malonate are combined with 50 ml of ethanol, then 28 ml 1N sodium hydroxide solution are added and the mixture is stirred overnight at RT. The next day another 28 ml of 1N sodium hydroxide solution are added and the mixture is refluxed for 6 h. After cooling to RT 50 ml 1N hydrochloric acid are added and the mixture is extracted with DCM. The phases are separated using a phase transfer cartridge. The filtrate is evaporated down i. V.

후처리

  1. temperaturethe mixture is refluxed for 6 h
  2. additionare added
  3. extractionthe mixture is extracted with DCM
  4. customThe phases are separated
  5. customThe filtrate is evaporated down i

출처 및 근거

ORD 기록
ord-2acfb75b7cfa407fa6d966a68c38ed75
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772323B2

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