Ethyl Acetate → HCID 178519659, Verbindung

HRID 2164620Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2164620
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([C:11]1[CH:16]=[C:15]([Cl:17])[C:14]([N:18]=[C:19]2[NH:23][CH2:22][CH2:21][NH:20]2)=[C:13]([Cl:24])[CH:12]=1)(OC)=[O:8].C(OCC)(=O)C>O1CCCC1>[Cl:24][C:13]1[CH:12]=[C:11]([CH2:7][OH:8])[CH:16]=[C:15]([Cl:17])[C:14]=1[N:18]=[C:19]1[NH:20][CH2:21][CH2:22][NH:23]1

Komponenten

5

Edukt 3

HCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 1784980442-(4-Carbomethoxy-2,6-dichlorophenylimino)imidazolidine

Produkt 1

HCID 178519659HCID 178519659, VerbindungAusbeute 48,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Lithium aluminium hydride (300 mg, 7.9 mM) was added to a stirred suspension of 2-(4-carbomethoxy-2,6-dichlorophenylimino)imidazolidine (750 mg, 2.6 mM) in dry tetrahydrofuran (50 ml) with stirring. The mixture was then stirred at room temperature for several hours after which time ethyl acetate was carefully added. The solvent was then removed under vacuum and water was added to the residue. After basification with dilute sodium hydroxide the aqueous mixture was extracted several times with ethyl acetate. The extract (750 mg) was dried and evaporated to give a solid which was recrystallised from isopropanol to give a white solid (330 mg) mp 208°-210° C.

Aufarbeitung

  1. additionwas carefully added
  2. customThe solvent was then removed under vacuum and water
  3. additionwas added to the residue
  4. extractionAfter basification with dilute sodium hydroxide the aqueous mixture was extracted several times with ethyl acetate
  5. extractionThe extract (750 mg)
  6. customwas dried
  7. customevaporated
  8. customto give a solid which
  9. customwas recrystallised from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-03d15d5525d64f13b9b5b2dbecec8919
Quelldatensatz
uspto-grants-1985_03
Patentnummer
US04505926

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