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Acetone → HCID 178434042, Verbindung

HRID 1022713
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1022713
[CH3:1]I.[NH2:3][C:4](=S)[CH2:5][C@H:6]1[C@H:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([Cl:20])[CH:14]=2)[O:11][CH2:10][CH2:9][N:8](C(OC(C)(C)C)=O)[CH2:7]1.[C:29](=[O:32])([O-])[O-:30].[K+].[K+].[C:35]([NH:38][NH2:39])(=O)[CH3:36].C(=O)([O-])O.[Na+].[CH3:45][C:46]([CH3:48])=O>>[Cl:20][C:15]1[CH:14]=[C:13]([C@@H:12]2[O:11][CH2:10][CH2:9][N:8]([C:29]([O:30][C:46]([CH3:48])([CH3:1])[CH3:45])=[O:32])[CH2:7][C@H:6]2[CH2:5][C:4]2[NH:3][C:35]([CH3:36])=[N:38][N:39]=2)[CH:18]=[CH:17][C:16]=1[Cl:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 6

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 14039AcetohydrazideHCID 516892Sodium BicarbonateHCID 86663871tert-butyl (6R,7R)-6-(2-amino-2-thioxoethyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

Produkt 1

HCID 178434042
HCID 178434042, Verbindung
Ausbeute 79 %

Versuchsvorschrift

Methyl iodide (0.214 mL, 3.43 mmol) was added to a suspension of tert-butyl (6R,7R)-6-(2-amino-2-thioxoethyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (288 mg, 0.69 mmol) and potassium carbonate (142 mg, 1.03 mmol) in acetone (5 mL) at room temperature. The reaction mixture was stirred at room temperature for 4 hr, and concentrated under reduced pressure. To the residue was added aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was dissolved in toluene (5 ml), acetohydrazide (61.1 mg, 0.82 mmol) was added, and the mixture was stirred at 120° C. overnight while using a Dean-Stark trap. To the reaction mixture was added aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (241 mg, 0.545 mmol, 79%).

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added aqueous sodium hydrogen carbonate solution
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. dissolutionThe residue was dissolved in toluene (5 ml)
  8. stirringthe mixture was stirred at 120° C. overnight
  9. extractionthe mixture was extracted with ethyl acetate
  10. washThe extract was washed with brine
  11. dry with materialdried over anhydrous sodium sulfate
  12. customThe solvent was evaporated under reduced pressure
  13. customThe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-0dc2c02fac124c96bbb19acd3b653633
Quelldatensatz
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08722662B2

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