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Aminoisobutyric acid → HCID 22313664, 화합물

HRID 965886
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HRID 965886 반응식
C([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](Cl)=[O:12])(=O)C.[CH2:14](N(C(C)C)C(C)C)C.[CH3:23][C:24]([C:27]([OH:29])=[O:28])([CH3:26])[NH2:25]>C1(C)C=CC=CC=1>[OH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]([NH:25][C:24]([CH3:26])([CH3:23])[C:27]([O:29][CH3:14])=[O:28])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6119Aminoisobutyric acidHCID 796682-Acetoxybenzoyl chlorideHCID 81531Diisopropylethylamine

생성물 1

HCID 22313664HCID 22313664, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a solution of 2-(chlorocarbonyl)phenyl acetate (20 mmol, 3.96 g) in toluene (50 ml) were N-ethyl-N,N-diisopropylamine (22 mmol, 2.84 g) and 2-methylalanine (22 mmol, 2.27 g) added. After stirring the reaction mixture at room temperature overnight, the mixture was diluted with 250 ml toluene and was washed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml). The organic phase was dried over Na2SO4 and concentrated under reduced pressure. The residue was dissolved in MeOH (50 mL) and 3 drops of conc. H2SO4 were added. The mixture was refluxed for 2 hours and concentrated under reduced pressure. The residue was dissolved in 250 mL EtOAc and washed with sat. NaHCO3/aq (250 ml) and sat. NaCl/aq (250 ml). The organic phase was dried over Na2SO4 and concentrated at reduced pressure. The resulting crude material was used without further purification.

후처리

  1. additionadded
  2. washwas washed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml)
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe residue was dissolved in MeOH (50 mL)
  6. addition3 drops of conc. H2SO4 were added
  7. temperatureThe mixture was refluxed for 2 hours
  8. concentrationconcentrated under reduced pressure
  9. dissolutionThe residue was dissolved in 250 mL EtOAc
  10. washwashed with sat. NaHCO3/aq (250 ml) and sat. NaCl/aq (250 ml)
  11. dry with materialThe organic phase was dried over Na2SO4
  12. concentrationconcentrated at reduced pressure
  13. customThe resulting crude material was used without further purification

출처 및 근거

ORD 기록
ord-e7a9c8e32194437fb44bca518ae3b9d7
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06951874B2

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