1,2-Dichloroethane → HCID 54297219, Verbindung

HRID 1683053Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1683053
C([N:8]1[CH2:26][CH2:25][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[C:14](=[O:23])[NH:13][C:12]2=[O:24])[CH2:10][CH2:9]1)C1C=CC=CC=1.ClCCCl.ClC(OC(Cl)C)=O>CO>[F:22][C:19]1[CH:20]=[CH:21][C:16]([N:15]2[C:11]3([CH2:10][CH2:9][NH:8][CH2:26][CH2:25]3)[C:12](=[O:24])[NH:13][C:14]2=[O:23])=[CH:17][CH:18]=1

Komponenten

5

Edukt 3

HCID 111,2-DichloroethaneHCID 5213051-Chloroethyl chloroformateHCID 53759290HCID 53759290, Verbindung

Produkt 1

HCID 54297219HCID 54297219, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Combine 8-benzyl-1-(4-fluoro-phenyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione (10 mmol) and 1,2-dichloroethane (70 mL). Cool using an ice bath. Add in dropwise fashion, 1-chloroethyl chloroformate (48.6 mmol). Warm to ambient temperature and maintain for 1 h. Extract using saturated NaHCO3 (120 mL). Extract the aqueous phase using dichloromethane (120 mL). Combine the organic layers, extract with saturated NaCl, dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Add anhydrous methanol (70 mL) and heat at reflux for 1 h. Concentrate in vacuo to obtain a residue and purify to obtain the title compound.

Aufarbeitung

  1. temperatureCool
  2. temperaturemaintain for 1 h
  3. extractionExtract
  4. extractionExtract the aqueous phase
  5. extractionCombine the organic layers, extract with saturated NaCl
  6. dry with materialdry over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo
  9. customto obtain a residue
  10. temperatureat reflux for 1 h
  11. concentrationConcentrate in vacuo
  12. customto obtain a residue
  13. custompurify

Quellen und Nachweise

ORD-Eintrag
ord-5cb933a4d7fd476ea85a5958d8dbbc79
Quelldatensatz
uspto-grants-1997_06
Patentnummer
US05635510

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