Hydrochloric Acid → 4-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

HRID 1619965노트

반응식

HRID 1619965 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:25])[CH:16]([CH:18](C(O)=O)[C:19]([OH:21])=[O:20])[CH3:17])=[CH:11][C:10]=1[OH:26])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)COCCO.COC.C(OC(C)C)(C)C.Cl>O>[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:25])[CH:16]([CH3:17])[CH2:18][C:19]([OH:21])=[O:20])=[CH:11][C:10]=1[OH:26])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 212256572-(2-Hydroxyethoxy)ethanol;methoxymethaneHCID 674670302-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

생성물 1

HCID 674661774-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

78.9 g (220.8 mmol) 2-[2-(4-benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid are combined with 200 ml diethyleneglycol-dimethylether and stirred for 3 h at 140° C. The mixture is combined with water and diisopropylether, then it is adjusted with 6N hydrochloric acid to pH=2 and extracted with DCM. The org. phase is separated off and dried on magnesium sulphate, then the solv. is eliminated by rotary evaporation i.V., the residue is stirred with diisopropylether and filtered off.

후처리

  1. extractionextracted with DCM
  2. customphase is separated off
  3. customdried on magnesium sulphate
  4. stirring, the residue is stirred with diisopropylether
  5. filtrationfiltered off

출처 및 근거

ORD 기록
ord-c9736f84cf7f46008f3683e08e20853f
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772323B2

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