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Aminoisobutyric acid → HCID 22313664、化合物

HRID 496184
ノート
印刷プレビュー

反応式

HRID 496184 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6119Aminoisobutyric acidHCID 796682-Acetoxybenzoyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 22313664HCID 22313664、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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
  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

出典と根拠

ORDレコード
ord-2f1222094bdb4ddfa7c4d99a2decd457
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06943188B2

反応ノート

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